CN107459549A - A kind of deflazacort fast reaction technique and production system - Google Patents
A kind of deflazacort fast reaction technique and production system Download PDFInfo
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- CN107459549A CN107459549A CN201710737537.XA CN201710737537A CN107459549A CN 107459549 A CN107459549 A CN 107459549A CN 201710737537 A CN201710737537 A CN 201710737537A CN 107459549 A CN107459549 A CN 107459549A
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 85
- FBHSPRKOSMHSIF-GRMWVWQJSA-N deflazacort Chemical compound C1CC2=CC(=O)C=C[C@]2(C)[C@@H]2[C@@H]1[C@@H]1C[C@H]3OC(C)=N[C@@]3(C(=O)COC(=O)C)[C@@]1(C)C[C@@H]2O FBHSPRKOSMHSIF-GRMWVWQJSA-N 0.000 title claims abstract description 47
- 229960001145 deflazacort Drugs 0.000 title claims abstract description 47
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 21
- 239000011229 interlayer Substances 0.000 claims abstract description 13
- 230000008569 process Effects 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 93
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 74
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 49
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 48
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 40
- 230000007704 transition Effects 0.000 claims description 40
- 229960000583 acetic acid Drugs 0.000 claims description 36
- 239000012362 glacial acetic acid Substances 0.000 claims description 34
- 238000001914 filtration Methods 0.000 claims description 33
- 238000003756 stirring Methods 0.000 claims description 33
- 239000000243 solution Substances 0.000 claims description 32
- 238000005352 clarification Methods 0.000 claims description 28
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims description 23
- 229910052740 iodine Inorganic materials 0.000 claims description 23
- 239000011630 iodine Substances 0.000 claims description 23
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 239000000413 hydrolysate Substances 0.000 claims description 20
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 18
- 239000012043 crude product Substances 0.000 claims description 16
- 239000000543 intermediate Substances 0.000 claims description 16
- 238000010792 warming Methods 0.000 claims description 16
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 238000001816 cooling Methods 0.000 claims description 14
- 239000000047 product Substances 0.000 claims description 13
- 239000011265 semifinished product Substances 0.000 claims description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 12
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 claims description 12
- 239000000126 substance Substances 0.000 claims description 11
- 229910021529 ammonia Inorganic materials 0.000 claims description 9
- 238000002425 crystallisation Methods 0.000 claims description 9
- 230000008025 crystallization Effects 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 9
- SCVFZCLFOSHCOH-UHFFFAOYSA-M potassium acetate Chemical compound [K+].CC([O-])=O SCVFZCLFOSHCOH-UHFFFAOYSA-M 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- WWILHZQYNPQALT-UHFFFAOYSA-N 2-methyl-2-morpholin-4-ylpropanal Chemical compound O=CC(C)(C)N1CCOCC1 WWILHZQYNPQALT-UHFFFAOYSA-N 0.000 claims description 7
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 7
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 7
- 229910052796 boron Inorganic materials 0.000 claims description 7
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 7
- 239000000292 calcium oxide Substances 0.000 claims description 7
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 7
- 238000006073 displacement reaction Methods 0.000 claims description 7
- 229910052739 hydrogen Inorganic materials 0.000 claims description 7
- 239000001257 hydrogen Substances 0.000 claims description 7
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims description 7
- 238000012423 maintenance Methods 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 235000011056 potassium acetate Nutrition 0.000 claims description 7
- 238000011084 recovery Methods 0.000 claims description 7
- 239000011734 sodium Substances 0.000 claims description 7
- 229910052708 sodium Inorganic materials 0.000 claims description 7
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 6
- 150000008064 anhydrides Chemical class 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 238000011049 filling Methods 0.000 claims description 5
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 claims description 5
- 230000003068 static effect Effects 0.000 claims description 5
- 150000004075 acetic anhydrides Chemical class 0.000 claims description 4
- 238000005119 centrifugation Methods 0.000 claims description 4
- -1 dichloromethanes Alkane Chemical class 0.000 claims description 4
- 238000000967 suction filtration Methods 0.000 claims description 4
- 230000002045 lasting effect Effects 0.000 claims description 3
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical class [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 230000009466 transformation Effects 0.000 claims description 3
- WFJRIDQGVSJLLH-UHFFFAOYSA-N methyl n-aminocarbamate Chemical class COC(=O)NN WFJRIDQGVSJLLH-UHFFFAOYSA-N 0.000 claims description 2
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 claims 2
- 239000002253 acid Substances 0.000 claims 1
- 150000007513 acids Chemical class 0.000 claims 1
- 150000002576 ketones Chemical class 0.000 claims 1
- 150000004702 methyl esters Chemical class 0.000 claims 1
- 230000035484 reaction time Effects 0.000 abstract description 2
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 description 12
- 238000010586 diagram Methods 0.000 description 8
- TZIHFWKZFHZASV-UHFFFAOYSA-N methyl formate Chemical compound COC=O TZIHFWKZFHZASV-UHFFFAOYSA-N 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 7
- 238000007789 sealing Methods 0.000 description 7
- 239000000498 cooling water Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 230000036632 reaction speed Effects 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 239000003610 charcoal Substances 0.000 description 4
- 125000000717 hydrazino group Chemical group [H]N([*])N([H])[H] 0.000 description 4
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 4
- 239000003960 organic solvent Substances 0.000 description 4
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 229960005205 prednisolone Drugs 0.000 description 3
- OIGNJSKKLXVSLS-VWUMJDOOSA-N prednisolone Chemical compound O=C1C=C[C@]2(C)[C@H]3[C@@H](O)C[C@](C)([C@@](CC4)(O)C(=O)CO)[C@@H]4[C@@H]3CCC2=C1 OIGNJSKKLXVSLS-VWUMJDOOSA-N 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 230000004044 response Effects 0.000 description 3
- 239000000052 vinegar Substances 0.000 description 3
- 235000021419 vinegar Nutrition 0.000 description 3
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- DTQVDTLACAAQTR-UHFFFAOYSA-N Trifluoroacetic acid Chemical compound OC(=O)C(F)(F)F DTQVDTLACAAQTR-UHFFFAOYSA-N 0.000 description 2
- 239000003377 acid catalyst Substances 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 238000009958 sewing Methods 0.000 description 2
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 description 1
- NMPCHDUPOXAUDX-UHFFFAOYSA-N CC1OC(CC(C(CC2)C3C(C)(C=C4)C2=CC4=O)C2(C)CCC3O)C2(C(C)=O)N1 Chemical compound CC1OC(CC(C(CC2)C3C(C)(C=C4)C2=CC4=O)C2(C)CCC3O)C2(C(C)=O)N1 NMPCHDUPOXAUDX-UHFFFAOYSA-N 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- 150000008065 acid anhydrides Chemical class 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- AEMFNILZOJDQLW-QAGGRKNESA-N androst-4-ene-3,17-dione Chemical compound O=C1CC[C@]2(C)[C@H]3CC[C@](C)(C(CC4)=O)[C@@H]4[C@@H]3CCC2=C1 AEMFNILZOJDQLW-QAGGRKNESA-N 0.000 description 1
- 229960005471 androstenedione Drugs 0.000 description 1
- AEMFNILZOJDQLW-UHFFFAOYSA-N androstenedione Natural products O=C1CCC2(C)C3CCC(C)(C(CC4)=O)C4C3CCC2=C1 AEMFNILZOJDQLW-UHFFFAOYSA-N 0.000 description 1
- 230000003266 anti-allergic effect Effects 0.000 description 1
- 230000003110 anti-inflammatory effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000003246 corticosteroid Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 125000003963 dichloro group Chemical group Cl* 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000005304 joining Methods 0.000 description 1
- 239000012567 medical material Substances 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- LYGJENNIWJXYER-UHFFFAOYSA-N nitromethane Chemical compound C[N+]([O-])=O LYGJENNIWJXYER-UHFFFAOYSA-N 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000012429 reaction media Substances 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 235000002639 sodium chloride Nutrition 0.000 description 1
- 230000002459 sustained effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07J—STEROIDS
- C07J71/00—Steroids in which the cyclopenta(a)hydrophenanthrene skeleton is condensed with a heterocyclic ring
- C07J71/0036—Nitrogen-containing hetero ring
- C07J71/0057—Nitrogen and oxygen
- C07J71/0068—Nitrogen and oxygen at position 16(17)
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Mixers Of The Rotary Stirring Type (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of deflazacort fast reaction technique and production system, production system includes reactor, elutriation kettle, spin-on filter device, concentration kettle, drying plant, the decolouring kettle being connected with each other according to process, reactor includes tank body, and tank wall is provided with interlayer cavity；Temperature adjustment pipe is provided with tank body；Center is provided with agitating shaft in tank body；Agitating shaft upper end connects magnetic couple rotating device, and lower end is provided with agitator arm；Agitating shaft is provided with rotating cylinder；Rotating cylinder is provided with buoyancy impeller；Buoyancy impeller upper end is provided with lifting disk；Lifting disk is provided with circular hole；Treatment hole is uniformly provided with lifting disk；Rotating cylinder outer wall is provided with vertical chute；The hub interior wall of buoyancy impeller is provided with roller bearing；The swivelling cover upper end of agitator arm is provided with upper keypad；Rotating cylinder lower end is provided with lower keypad.The production system and technique can realize the multi-party bit flow of reaction solution, reduce the reaction time of each step of deflazacort, realize the quick production of deflazacort.
Description
Technical field
The invention belongs to chemical technology field, specially a kind of deflazacort fast reaction technique and production system.
Background technology
Deflazacort is mainly used in corticosteroid medical material and intermediate, is a kind of white or off-white color crystalline powder,
With anti-inflammatory, anti-allergic effects, equivalent to 10~20 times of prednisolone, for hypocorticoidism, LADA
Disease, anaphylactia and disease in the blood system etc..When traditional deflazacort produces, due to needing to react using multi-step chemical
Produced, and raw material poor fluidity in reaction solution, cause each chemical time longer, cause the life of deflazacort
Produce the time to grow very much, production efficiency is low.
The content of the invention
It is an object of the invention to for problem above, there is provided a kind of quick production system of deflazacort, in reactor
Agitating device can realize the multi-party bit flow of reaction solution, reduce the reaction time of each step of deflazacort, realize deflazacort
Quick production.
To realize the purpose, the technical solution adopted by the present invention is：A kind of quick production system of deflazacort, it include according to
Reactor, elutriation kettle, spin-on filter device, concentration kettle, drying plant, the decolouring kettle of process interconnection, the reactor bag
Tank body 1 is included, interlayer cavity is provided with the outer wall of tank body 1；Vertical temperature adjustment pipe 9 is evenly arranged with the tank body 1；The tank body 1
Inside it is provided centrally with agitating shaft 2；The upper end of agitating shaft 2 connects magnetic couple rotating device 3 by static seal mode, and lower end is set
It is equipped with agitator arm 7；Rotatable rotating cylinder 4 is provided with the agitating shaft 2；Be provided with the rotating cylinder 4 can oscilaltion simultaneously
The buoyancy impeller 6 of rotation；The upper end of buoyancy impeller 6 is provided with the lifting disk 5 that can be moved up and down with buoyancy impeller 6；The liter
The circular hole 51 for being socketed temperature adjustment pipe is provided with drop disk 5；Treatment hole is evenly arranged with the lifting disk 5；Outside the rotating cylinder 4
Vertical chute 41 is evenly arranged with wall；It is evenly arranged with and is used for and vertical chute on the inwall of block set 64 of the buoyancy impeller 6
41 roller bearings 61 coordinated；The upper end of swivelling cover 71 of the agitator arm 7 is uniformly provided with vertical upper keypad 72 in a ring；It is described
The lower end of rotating cylinder 4 is provided with the lower keypad 42 coordinated with upper keypad 72.
Further, the agitator arm 7 includes the blade 73 being uniformly arranged on swivelling cover 71；71 sets of the swivelling cover
It is connected on agitating shaft 2；The inwall of swivelling cover 71 is evenly arranged with vertical interior keypad 74；The lower end of agitating shaft 2 is uniformly set
It is equipped with the swinging plate 21 coordinated with interior keypad 74.
Further, the height of the swinging plate 21 is less than the height of the inwall of swivelling cover 71.
Further, the upper surface of block set 64 is uniformly inlaid with rotatable ball 62.
Further, it is additionally provided with the arc scraper plate 63 moved in vertical chute 41 on the inwall of block set 64.
Further, fixed impeller 52 is also evenly arranged with the lifting disk 5.
Further, U-shaped conduit 93 is provided with the temperature adjustment pipe 9；Set between the U-shaped conduit 93 and temperature adjustment pipe 9
There is heat filling 94；The U-shaped conduit 93；The temperature adjustment pipe 9 includes hot-water line 91 and condenser pipe 92；The hot-water line 91 and cold
Solidifying pipe 92 alternates setting.
Further, the interlayer cavity includes the heating chamber 81 and cooling chamber 82 at interlaced interval.
It is a further object to provide a kind of deflazacort using above-mentioned Quick response sewing system to produce work
Skill, the technique is by using the production time that deflazacort is substantially shorter after above-mentioned production system.
This technique includes following preparation process：
It is prepared by oxide：80-120 part moulds dehydrogen substance, 150-250 parts glacial acetic acid, 20-50 part chromium are added in a kettle
Acid anhydride, 8-20 part manganese acetates, temperature is 35~38 DEG C in maintenance reaction kettle, and control reactor agitator shaft speed is by 30-180r/min
Alternate transition, wherein lowest speed continue 5 minutes every time, and most high speed continues 2 minutes every time, after stirring reaction 2-3 hours, add
After the sodium hydroxide solution that 1500-2000 parts mass percentage concentration is 5.4% carries out elutriation, centrifugal filtration obtains oxide；
Reaction equation is：
It is prepared by protection：80-100 parts oxide, 30-70 parts glacial acetic acid, 1200-2000 parts are added in a kettle
Water, 20-60 part methyl hydrazinocarboxylates, it is 20~25 DEG C to control temperature of reaction kettle, and control reactor agitator shaft speed is by 30-
240r/min alternate transitions, wherein lowest speed continue 5 minutes every time, and most high speed continues 3 minutes every time, after reacting 4-6 hours, from
The heart filters to obtain protection；
Reaction equation is：
It is prepared by closed loop hydrolysate：100-140 parts protection, 600-1000 part chloroforms are added in a kettle,
It is 25~28 DEG C to control reactor temperature, persistently stirs and is passed through ammonia, and control reactor agitator shaft speed is by 30-300r/
Min alternate transitions, wherein lowest speed continue 5 minutes every time, and most high speed continues 5 minutes every time, are obtained after reaction 8-12 hours middle
Thing；
800-1000 parts intermediate is pumped into washing kettle, after being washed with water once, is transferred in reactor, is added
60-100 part aceticanhydrides, 80-120 part glacial acetic acid, control reactor agitator shaft speed is by 30-180r/min alternate transitions, wherein most
Low speed continues 5 minutes every time, and most high speed continues 1 minute every time, reacts 0.8-1 hours, after negative pressure is concentrated and dried, then in reactor
Middle addition 900-1200 part methanol, controlling reactor temperature, control is anti-in order in ± 1 DEG C, 6-9 part boron hydrogen sodium to be added in four times
Kettle agitator shaft speed is answered to continue 4 minutes every time by 20-80r/min alternate transitions, wherein lowest speed, most high speed continues 1 point every time
Clock, 2-3 hours are reacted, add 8-12 parts glacial acetic acid and neutralize, negative pressure concentration falls methanol, adds 1500-1800 parts quality hundred
The ammonium hydrogen sulfate aqueous solution and 80-120 part formaldehyde for dividing concentration to be 10%, 40~45 DEG C of reaction 5-7 hours are warming up to, then are down to 5
~10 DEG C, centrifugal filtration, neutrality is washed to, dries to obtain crude product；
Above-mentioned crude product is put into decolouring kettle, 60-90 part dichloromethane is added, 400-600 part methanol dissolved clarifications, adds 4-
6 parts of activated carbons, decolouring 0.5-1.5 hours, it is put into after filtering in concentration kettle, negative pressure concentration, freezes crystallization, centrifuging to close
Cyclizing hydrolysis thing fine work；
Reaction equation is：
Upper Iod R：75 parts of hydrolysate fine work are put into reactor, add 120-160 part methanol, 120-
160 parts of dichloromethane, dissolved clarification is stirred, add 20-45 part calcium oxide, dissolved clarification is stirred at 25~30 DEG C, 50-80 parts iodine is added dropwise
Enter in reactor, control iodine, which is added dropwise, continues 0.8-1.2 hours, and control reactor agitator shaft speed is alternately turned by 30-120r/min
Become, wherein lowest speed continues 3 minutes every time, and most high speed continues 3 minutes every time；It is that 20% glacial acetic acid is molten to add mass percentage concentration
Liquid carries out elutriation, and centrifugal filtration must go up iodine thing；
Reaction equation is：
Displacement reaction：Described 125 parts upper iodine things are put into reactor, 600-800 part acetone is added, adds 70-
90 parts of potassium acetates, lasting stirring, lead to nitrogen, are warming up to 56~58 DEG C, control reactor agitator shaft speed is handed over by 30-180r/min
For transformation, wherein lowest speed continues 5 minutes every time, and most high speed continues 1 minute every time, reacts 1.5-3 hours, controls less than 50 DEG C
Concentration and recovery acetone adds 900-1200 parts water and carries out elutriation to being distillated without acetone, is cooled to 20-25 DEG C, centrifuge dripping obtains half
Finished product；
The semi-finished product are put into decolouring kettle, 300-500 part methanol is added, 100-200 part dichloromethane dissolved clarifications, adds
Enter 5-10 part activated carbon decolorizings, suction filtration is concentrated into small size, centrifuges, dries to obtain deflazacort finished product；
Reaction equation is：
Preferably, a kind of deflazacort fast reaction technique includes following preparation process：
It is prepared by oxide：100 parts of mould dehydrogen substances, 200 parts of glacial acetic acid, 40 parts of chromic anhydrides, 14 portions of vinegar are added in a kettle
Sour manganese, temperature is 35~38 DEG C in maintenance reaction kettle, control reactor agitator shaft speed by 30-180r/min alternate transitions, its
Middle lowest speed continues 5 minutes every time, and most high speed continues 2 minutes every time, after stirring reaction 2-3 hours, adds 1650 parts of quality
After the sodium hydroxide solution that percentage concentration is 5.4% carries out elutriation, centrifugal filtration obtains oxide；
It is prepared by protection：98 parts of oxides, 50 parts of glacial acetic acid, 1500 parts of water, 40 parts of diazanyls are added in a kettle
Methyl formate, it is 20~25 DEG C to control temperature of reaction kettle, control reactor agitator shaft speed by 30-240r/min alternate transitions,
Wherein lowest speed continues 5 minutes every time, and most high speed continues 3 minutes every time, and after reacting 4-6 hours, centrifugal filtration obtains protection.
It is prepared by closed loop hydrolysate：120 parts of protection, 800 parts of chloroforms are added in a kettle, control reactor
Interior temperature is 25~28 DEG C, persistently stirs and is passed through ammonia, and control reactor agitator shaft speed is alternately turned by 30-300r/min
Become, wherein lowest speed continues 5 minutes every time, and most high speed continues 5 minutes every time, and reaction obtains intermediate after 10 hours；
940 parts of intermediates are pumped into washing kettle, after being washed with water once, are transferred in reactor, add 80 parts
Aceticanhydride, 100 parts of glacial acetic acid, control reactor agitator shaft speed are continued every time by 30-180r/min alternate transitions, wherein lowest speed
5 minutes, most high speed continued 1 minute every time, reacted 1 hour, after negative pressure is concentrated and dried, then added 1000 parts of first in a kettle
Alcohol, it is 0 DEG C to control reactor temperature, and 7.5 parts of boron hydrogen sodium are added in four times, and control reactor agitator shaft speed is by 20-
80r/min alternate transitions, wherein lowest speed continue 4 minutes every time, and most high speed continues 1 minute every time, after reacting 2-3 hours, add
Enter 10 parts of glacial acetic acid to neutralize, negative pressure concentration falls methanol, adds the ammonium hydrogen sulfate water that 1600 parts of mass percentage concentrations are 10%
Solution and 100 parts of formaldehyde, it is warming up to 40~45 DEG C and reacts 6 hours, then be down to 6 DEG C, centrifugal filtration, is washed to neutrality, dries
Crude product；
Above-mentioned crude product is put into decolouring kettle, 80 parts of dichloromethane is added, 500 parts of methanol dissolved clarifications, adds 5 parts of activity
Charcoal, decolourize 1 hour, be put into after filtering in concentration kettle, negative pressure concentration, freeze crystallization, centrifuge to obtain closed loop hydrolysate fine work；
Upper Iod R：The hydrolysate fine work is put into reactor, adds 140 parts of methanol, 140 parts of dichloromethanes
Alkane, dissolved clarification is stirred, add 35 parts of calcium oxide, stir dissolved clarification at 25~30 DEG C, 70 parts of iodine are added dropwise in reactor, control is anti-
Kettle agitator shaft speed is answered to continue 3 minutes every time by 30-120r/min alternate transitions, wherein lowest speed, most high speed continues 3 points every time
Clock, control iodine, which is added dropwise, continues 1 hour, and it is that 20% glacial acetic acid solution carries out elutriation, centrifugal filtration to add 420 parts of mass percentage concentrations
Iodine thing must be gone up；
Displacement reaction：The upper iodine thing is put into reactor, 700 parts of acetone is added, 84 parts of potassium acetates, persistently stirs
Mix, lead to nitrogen, be warming up to 56~58 DEG C, control reactor agitator shaft speed is by 30-180r/min alternate transitions, wherein lowest speed
Continue 5 minutes every time, most high speed continues 1 minute every time, reacts 2 hours, controls less than 50 DEG C concentration and recovery acetone to without acetone
Distillate, add 1000 parts of water and carry out elutriation, be cooled to 20-25 DEG C, centrifuge dripping obtains semi-finished product；
The semi-finished product are put into decolouring kettle, 420 parts of methanol is added, 140 parts of dichloromethane dissolved clarifications, adds 7 parts of work
Property carbon decoloring, filter concentration, centrifugation, dry to obtain deflazacort finished product.
Beneficial effects of the present invention：
1st, reactor passes through magnetic couple rotating dress using static seal mode in the Quick response sewing system in the present invention
Control agitator rotation is put, the sealing property of reactor is substantially increased, effectively prevents outside air from entering reactor, influence
The reaction efficiency of chemical reaction, the production purity of deflazacort is improved, improves production security.
2nd, as needed rotating cylinder can be driven to be rotated in the agitator arm rotary course in the present invention, so as to drive buoyancy
Impeller is rotated and lifted, and then controls the oscilaltion of lifting disk, and the Quick uniform for realizing each reactant in solution connects
Touch, improve chemical reaction velocity, reduce chemical time, through our company's actual production statistics, using this processing technology
During with production system, relative to traditional deflazacort processing technology, the present invention can shorten 40-50% process time.
3rd, the present invention in lifting disk can automatic oscilaltion, drive tank in reaction solution it is quick up and down stir, improve reaction
Speed, while the circular hole on lifting disk can realize the automatic cleaning to heterotherm tube, and the reaction joining thing adhered to thereon is removed
Fall；Buoyancy impeller can not only realize rotary motion simultaneously but also realize oscilaltion campaign, substantially increase stirring for solution
Property, improve the chemical reaction uniformity and reaction speed of solution.
4th, the heterotherm tube that uses is evenly distributed in tank body in the present invention, coordinates the interlayer cavity of outer wall, external heat in realization
And cooling, ramp rates are substantially increased, while flowing, hot water are individually further isolated using circulating hot water and circulating water
Pipe and condenser pipe are arranged at intervals, and interlayer cavity also using the setting that colds and heat succeed each other, greatly shortens ramp rates, shortens wholeization
The time reacted and required needed for alternating temperature is learned, improves the speed of production of deflazacort.
5th, the present invention being slowly stirred only with agitator arm as needed, agitator arm, buoyancy leaf can also be realized
The quick rotation of wheel and the fast lifting of lifting disk, using flexible is changeable, is applicable to a variety of chemical reactions for needing quick changeable temperature,
Improve the scope of application and reaction speed of reactor.
Brief description of the drawings
Fig. 1 is the processing process figure of deflazacort in the present invention.
Fig. 2 is reactor internal structure schematic diagram in the present invention.
Fig. 3 is local A mplifying structure schematic diagrams in Fig. 2.
Fig. 4 is reactor overlooking the structure diagram in the present invention.
Fig. 5 is the lower surface structural representation of rotating cylinder.
Fig. 6 is the end view that buoyancy impeller is arranged on rotating cylinder.
Fig. 7 is the cross section structure diagram that buoyancy impeller is arranged on rotating cylinder.
Fig. 8 is blade structure schematic diagram.
Fig. 9 is agitator arm overlooking the structure diagram.
Figure 10 is agitator arm upward view.
Figure 11 is lifting disk structural representation.
Figure 12 is a specific embodiment schematic diagram of lifting disk.
Figure 13 is temperature adjustment tubular construction schematic diagram.
Figure 14 is deflazacort production technology material balance figure one.
Figure 15 is deflazacort production technology material balance figure two.
In figure：1st, tank body；2nd, agitating shaft；3rd, magnetic couple rotating device；4th, rotating cylinder；5th, lifting disk；6th, buoyancy impeller；7、
Agitator arm；8th, interlayer cavity；9th, temperature adjustment pipe；21st, swinging plate；41st, vertical chute；42nd, lower keypad；51st, circular hole；52nd, fixed leaf
Wheel；61st, roller bearing；62nd, ball；63rd, scraper plate；64th, block set；71st, swivelling cover；72nd, upper keypad；73rd, blade；74th, interior keypad；81、
Heating chamber；82nd, cooling chamber；91st, hot-water line；92nd, condenser pipe；93rd, U-shaped conduit；94th, heat filling.
Embodiment
In order that those skilled in the art more fully understand technical scheme, the present invention is entered below in conjunction with the accompanying drawings
Row is described in detail, and the description of this part is only exemplary and explanatory, should not there is any limitation to protection scope of the present invention
Effect.
As shown in Fig. 1-Figure 13, concrete structure of the invention is：A kind of quick production system of deflazacort, it is included according to work
Reactor, elutriation kettle, spin-on filter device, concentration kettle, drying plant, the decolouring kettle of sequence interconnection, the reactor include
Tank body 1, interlayer cavity 8 is provided with the outer wall of tank body 1；Vertical temperature adjustment pipe 9 is evenly arranged with the tank body 1；In the tank body 1
It is provided centrally with agitating shaft 2；The upper end of agitating shaft 2 connects magnetic couple rotating device 3 by static seal mode, and lower end is set
There is agitator arm 7；Rotatable rotating cylinder 4 is provided with the agitating shaft 2；Being provided with the rotating cylinder 4 oscilaltion and to revolve
The buoyancy impeller 6 turned；The upper end of buoyancy impeller 6 is provided with the lifting disk 5 that can be moved up and down with buoyancy impeller 6；The lifting
The circular hole 51 for being socketed temperature adjustment pipe 9 is provided with disk 5；Treatment hole is evenly arranged with the lifting disk 5；Outside the rotating cylinder 4
Vertical chute 41 is evenly arranged with wall；It is evenly arranged with and is used for and vertical chute on the inwall of block set 64 of the buoyancy impeller 6
41 roller bearings 61 coordinated；The upper end of swivelling cover 71 of the agitator arm 7 is uniformly provided with vertical upper keypad 72 in a ring；It is described
The lower end of rotating cylinder 4 is provided with the lower keypad 42 coordinated with upper keypad 72.
Preferably, the agitator arm 7 includes the blade 73 being uniformly arranged on swivelling cover 71；The swivelling cover 71 is socketed
On agitating shaft 2；The inwall of swivelling cover 71 is evenly arranged with vertical interior keypad 74；The lower end of agitating shaft 2 is uniformly arranged
There is the swinging plate 21 coordinated with interior keypad 74.
Preferably, the height of the swinging plate 21 is less than the height of the inwall of swivelling cover 71.
Preferably, the upper surface of block set 64 is uniformly inlaid with rotatable ball 62.
Preferably, it is additionally provided with the arc scraper plate 63 moved in vertical chute 41 on the inwall of block set 64.
Preferably, fixed impeller 52 is also evenly arranged with the lifting disk 5.
Preferably, U-shaped conduit 93 is provided with the temperature adjustment pipe 9；It is provided between the U-shaped conduit 93 and temperature adjustment pipe 9
Heat filling 94；The U-shaped conduit 93；The temperature adjustment pipe 9 includes hot-water line 91 and condenser pipe 92；The hot-water line 91 and condensation
Pipe 92 alternates setting.
Preferably, the interlayer cavity 8 includes the heating chamber 81 and cooling chamber 82 at interlaced interval.
Magnetic couple rotating device 3 uses magnetically-actuated, and magnetically-actuated is a kind of Novel transmission of the eighties exploitation
Sealing Technology.The critical component magnetic driver device of magnetic agitation reactor is that one kind utilizes permanent-magnet material to carry out coupled drive
Transmission device, that for changing tradition machinery sealing and packing seal can cross the dynamic sealing of axle sleeve or packing seal agitating shaft
Structure is static seal structure, and medium is completely in the annular seal space being made up of kettle with sealing cover body in kettle, is thoroughly solved and is filled out
Material sealing and mechanical seal because dynamic sealing and caused by the leakage problem that can not overcome, make absolutely not any leakage of reaction medium and dirt
Dye.It is the ideal device of the domestic chemical reaction carried out at present under high temperature, high pressure, particularly carries out inflammable, explosive, poisonous
The chemical reaction of medium, more show its superiority.
Magnetic couple rotating device 3 is started by control system, magnetic couple rotating device 3 drives agitating shaft by magnetic force
2 rotations, the swinging plate 21 of the lower end of agitating shaft 2 is stirred interior keypad 74 and rotated, so as to drive agitator arm 7 to rotate；When agitating shaft 2 revolves
When rotary speed is slow, agitator arm 7 rotates caused buoyancy and risen insufficient for agitator arm 7, therefore now only stirs
Impeller 7 rotates, and rotating cylinder 4, buoyancy impeller 6 can not rotate, and lifting disk 5 can not lift.
When the rotary speed of agitating shaft 2, which increases, make it that agitator arm 7 rotates caused buoyancy more than agitator arm deadweight, stir
To mix impeller 7 and rise certain distance, upper keypad 72 engages with the lower keypad 42 on rotating cylinder 4, and agitator arm 7 drives rotating cylinder 4 to rotate, by
It is fastened in the roller bearing 61 on buoyancy impeller 6 in vertical chute 41, therefore the rotation of rotating cylinder 4 drives buoyancy impeller 6 to rotate, when floating
Power impeller 6 rotate caused by buoyancy when being more than the deadweight of buoyancy impeller 6 and lifting disk 5, buoyancy impeller 6 start to rotate while
Rise, and promote lifting disk 5 and then to rise, when the rotary speed of agitating shaft 2 reduces, it is small that buoyancy impeller 6 rotates caused buoyancy
In the deadweight of buoyancy impeller 6 and lifting disk 5, buoyancy impeller is rotated while declining, and lifting disk 5 follows buoyancy impeller 6 to decline.
Treatment hole is evenly arranged with lifting disk 5, that is, reduces resistance of the liquid to lifting disk 5, while make it that lifting disk 5 is right
Reaction solution scrape up and down, improves the convective motion up and down of reaction solution；Lifting disk 5 can also be scraped to temperature adjustment pipe 9 simultaneously
Cleaning is wiped, material reaction on temperature adjustment pipe 9 is formed into sticky object scraped clean, ensures the heat transfer efficiency of temperature adjustment pipe 9.
Fixed impeller 52 can also be set on lifting disk 5, and fixed impeller 52 can cause local current to form small whirlpool, enter
One step improves the flow effect of reaction solution, improves reaction speed.
When the speed of agitating shaft 2 alternately changes from fast to slow, buoyancy impeller 6 and the reciprocal raising and lowering of lifting disk 5, together
When buoyancy impeller 6 rotate；So that the reaction solution in reactor produces the flowing in multiple orientation, reaction speed is greatly promoted
With reaction uniformity, while can cause chemical reaction process in caused heat be released rapidly, also improve interlayer cavity 8 and tune
Warming and cooling rate of the warm pipe 9 to reaction solution.
It has been uniformly arranged multiple temperature adjustment pipes 9 vertically in the inner chamber of reactor, has there is U-shaped conduit 93 in temperature adjustment pipe 9, it is U-shaped to lead
Pipe 93 connects thermal water source or cold water source, can greatly improve the warming and cooling rate of reaction solution in reactor, and it is accurate to improve chemical reaction
True property and reaction speed.
Interlayer cavity 8 in reactor is staggered using heating chamber 81 and cooling chamber 82, and user can add as needed
Hot chamber 81 is either passed through hot water or cooling water in cooling chamber 82, can also be passed through simultaneously in heating chamber 81 or cooling chamber 82
Hot water or cooling water.
Interlayer cavity 8 in reactor is staggered using heating chamber 81 and cooling chamber 82, when in use, during pyroreaction only
Hot water is passed through in heating chamber 81；Not water flowing in cooling chamber 82, during alternating temperature, when the hot water in heating chamber 81 is not returned also,
It can shift to an earlier date and cooling water is passed through in cooling chamber 82, improve ramp rates；During low-temp reaction, principle is same as above.
Temperature adjustment pipe 9 in reactor is staggered using hot-water line 91 and condenser pipe 92, and user can be as needed in heat
Hot water or cooling water are passed through in water pipe 91 or condenser pipe 92, hot water can also be passed through in hot-water line 91 and condenser pipe 92 simultaneously
Or cooling water.
Temperature adjustment pipe 9 in reactor is staggered using hot-water line 91 and condenser pipe 92, when reaction solution needs to be become by high temperature
For low temperature when, when the hot water in hot-water line 91 is not returned also, cooling water has been recycled into U-shaped conduit 93, right in advance
Reaction solution is cooled down, and substantially increases ramp rates；When reaction solution needs to be changed into high temperature from low temperature, principle is same as above.
Shown in reference picture 1, a kind of deflazacort production. art embodiment one：
It is prepared by oxide：80 parts of mould dehydrogen substances, 150 parts of glacial acetic acid, 20 parts of chromic anhydrides, 8 parts of acetic acid are added in a kettle
Manganese, temperature is 35~38 DEG C in maintenance reaction kettle, control reactor agitator shaft speed by 30-180r/min alternate transitions, wherein
Lowest speed continues 5 minutes every time, and most high speed continues 2 minutes every time, and stirring reaction adds 1500 parts of quality percentages after 2 hours
After the sodium hydroxide solution that concentration is 5.4% carries out elutriation, centrifugal filtration obtains oxide；
Reaction equation is：
It is prepared by protection：80 parts of oxides, 30 parts of glacial acetic acid, 1200 parts of water, 20 parts of diazanyls are added in a kettle
Methyl formate, it is 20~25 DEG C to control temperature of reaction kettle, control reactor agitator shaft speed by 30-240r/min alternate transitions,
Wherein lowest speed continues 5 minutes every time, and most high speed continues 3 minutes every time, and after reacting 4 hours, centrifugal filtration obtains protection；
Reaction equation is：
It is prepared by closed loop hydrolysate：100 parts of protection, 600 parts of chloroforms are added in a kettle, control reactor
Interior temperature is 25~28 DEG C, persistently stirs and is passed through ammonia, and control reactor agitator shaft speed is alternately turned by 30-300r/min
Become, wherein lowest speed continues 5 minutes every time, and most high speed continues 5 minutes every time, and reaction obtains intermediate after 8 hours；
800 parts of intermediates are pumped into washing kettle, after being washed with water once, are transferred in reactor, add 60 parts
Aceticanhydride, 80 parts of glacial acetic acid, control reactor agitator shaft speed continue 5 every time by 30-180r/min alternate transitions, wherein lowest speed
Minute, most high speed continues 1 minute every time, reacts 0.8 hour, after negative pressure is concentrated and dried, then adds 900 parts of first in a kettle
Alcohol, reactor temperature is controlled as in ± 1 DEG C, 6 parts of boron hydrogen sodium are added in four times, control reactor agitator shaft speed is by 20-
80r/min alternate transitions, wherein lowest speed continue 4 minutes every time, and most high speed continues 1 minute every time, react 2 hours, add 8 parts
Glacial acetic acid neutralizes, and negative pressure concentration falls methanol, add the ammonium hydrogen sulfate aqueous solution that 1500 parts of mass percentage concentrations are 10% and
80 parts of formaldehyde, it is warming up to 40~45 DEG C and reacts 5 hours, then be down to 5~10 DEG C, centrifugal filtration, is washed to neutrality, dries slightly
Product；
Above-mentioned crude product is put into decolouring kettle, 60 parts of dichloromethane is added, 400 parts of methanol dissolved clarifications, adds 4 parts of activity
Charcoal, decolourize 0.5 hour, be put into after filtering in concentration kettle, negative pressure concentration, freeze crystallization, centrifuge to obtain closed loop hydrolysate essence
Product；
Reaction equation is：
Upper Iod R：The hydrolysate fine work is put into reactor, adds 120 parts of methanol, 120 parts of dichloromethanes
Alkane, dissolved clarification is stirred, add 20 parts of calcium oxide, stir dissolved clarification at 25~30 DEG C, 50 parts of iodine are added dropwise in reactor, control iodine
Dropwise addition continues 0.8 hour, and control reactor agitator shaft speed continues 3 every time by 30-120r/min alternate transitions, wherein lowest speed
Minute, most high speed continues 3 minutes every time；It is that 20% glacial acetic acid solution carries out elutriation to add mass percentage concentration, and centrifugal filtration obtains
Upper iodine thing；
Reaction equation is：
Displacement reaction：The upper iodine thing is put into reactor, adds 600 parts of acetone, 70 parts of potassium acetates is added, holds
Continuous stirring, leads to nitrogen, is warming up to 56~58 DEG C, control reactor agitator shaft speed is by 30-180r/min alternate transitions, wherein most
Low speed continues 5 minutes every time, and most high speed continues 1 minute every time, reacts 1.5 hours, and less than 50 DEG C concentration and recovery acetone of control are extremely
Distillated without acetone, add 900 parts of water and carry out elutriation, be cooled to 20-25 DEG C, centrifuge dripping obtains semi-finished product；
The semi-finished product are put into decolouring kettle, 300 parts of methanol is added, 100 parts of dichloromethane dissolved clarifications, adds 5 parts of work
Property carbon decoloring, suction filtration be concentrated into small size, centrifuge, dry to obtain deflazacort finished product；
Reaction equation is：
Shown in reference picture 1, a kind of deflazacort fast reaction process example two：
It is prepared by oxide：120 parts of mould dehydrogen substances, 250 parts of glacial acetic acid, 50 parts of chromic anhydrides, 20 portions of vinegar are added in a kettle
Sour manganese, temperature is 35~38 DEG C in maintenance reaction kettle, control reactor agitator shaft speed by 30-180r/min alternate transitions, its
Middle lowest speed continues 5 minutes every time, and most high speed continues 2 minutes every time, and stirring reaction adds 2000 parts of quality hundred after 3 hours
After dividing the sodium hydroxide solution that concentration is 5.4% to carry out elutriation, centrifugal filtration obtains oxide；
It is prepared by protection：100 parts of oxides, 70 parts of glacial acetic acid, 2000 parts of water, 60 parts of diazanyls are added in a kettle
Methyl formate, it is 20~25 DEG C to control temperature of reaction kettle, control reactor agitator shaft speed by 30-240r/min alternate transitions,
Wherein lowest speed continues 5 minutes every time, and most high speed continues 3 minutes every time, and after reacting 6 hours, centrifugal filtration obtains protection；
It is prepared by closed loop hydrolysate：140 parts of protection, 1000 parts of chloroforms, control reaction are added in a kettle
Temperature in the kettle is 25~28 DEG C, persistently stirs and is passed through ammonia, and control reactor agitator shaft speed is alternately turned by 30-300r/min
Become, wherein lowest speed continues 5 minutes every time, and most high speed continues 5 minutes every time, and reaction obtains intermediate after 12 hours；
1000 parts of intermediates are pumped into washing kettle, after being washed with water once, are transferred in reactor, add 100
Part aceticanhydride, 120 parts of glacial acetic acid, control reactor agitator shaft speed are held every time by 30-180r/min alternate transitions, wherein lowest speed
Continuous 5 minutes, most high speed continues 1 minute every time, reacts 1 hour, after negative pressure is concentrated and dried, then adds 1200 parts of first in a kettle
Alcohol, reactor temperature is controlled as in ± 1 DEG C, 9 parts of boron hydrogen sodium are added in four times, control reactor agitator shaft speed is by 20-
80r/min alternate transitions, wherein lowest speed continue 4 minutes every time, and most high speed continues 1 minute every time, react 3 hours, add 12
Part glacial acetic acid neutralizes, and negative pressure concentration falls methanol, adds the ammonium hydrogen sulfate aqueous solution that 1800 parts of mass percentage concentrations are 10%
With 120 parts of formaldehyde, it is warming up to 40~45 DEG C and reacts 7 hours, then be down to 5~10 DEG C, centrifugal filtration, is washed to neutrality, dries
Crude product；
Above-mentioned crude product is put into decolouring kettle, 90 parts of dichloromethane is added, 600 parts of methanol dissolved clarifications, adds 6 parts of activity
Charcoal, decolourize 1.5 hours, be put into after filtering in concentration kettle, negative pressure concentration, freeze crystallization, centrifuge to obtain closed loop hydrolysate essence
Product；
Upper Iod R：The hydrolysate fine work is put into reactor, adds 160 parts of methanol, 160 parts of dichloromethanes
Alkane, dissolved clarification is stirred, add 45 parts of calcium oxide, stir dissolved clarification at 25~30 DEG C, 80 parts of iodine are added dropwise in reactor, control iodine
Dropwise addition continues 1.2 hours, and control reactor agitator shaft speed continues 3 every time by 30-120r/min alternate transitions, wherein lowest speed
Minute, most high speed continues 3 minutes every time；It is that 20% glacial acetic acid solution carries out elutriation to add mass percentage concentration, and centrifugal filtration obtains
Upper iodine thing；
Displacement reaction：The upper iodine thing is put into reactor, adds 800 parts of acetone, 90 parts of potassium acetates is added, holds
Continuous stirring, leads to nitrogen, is warming up to 56~58 DEG C, control reactor agitator shaft speed is by 30-180r/min alternate transitions, wherein most
Low speed continues 5 minutes every time, and most high speed continues 1 minute every time, reacts 3 hours, less than 50 DEG C concentration and recovery acetone of control to nothing
Acetone distillates, and adds 1200 parts of water and carries out elutriation, is cooled to 25 DEG C, centrifuge dripping obtains semi-finished product；
The semi-finished product are put into decolouring kettle, 500 parts of methanol is added, 200 parts of dichloromethane dissolved clarifications, adds 10 parts of work
Property carbon decoloring, suction filtration be concentrated into small size, centrifuge, dry to obtain deflazacort finished product；
As shown in figs. 14-15, a kind of deflazacort fast reaction process example three：
It is prepared by oxide：100 parts of mould dehydrogen substances, 200 parts of glacial acetic acid, 40 parts of chromic anhydrides, 14 portions of vinegar are added in a kettle
Sour manganese, temperature is 35~38 DEG C in maintenance reaction kettle, control reactor agitator shaft speed by 30-180r/min alternate transitions, its
Middle lowest speed continues 5 minutes every time, and most high speed continues 2 minutes every time, after stirring reaction 2-3 hours, adds 1650 parts of quality
After the sodium hydroxide solution that percentage concentration is 5.4% carries out elutriation, centrifugal filtration obtains oxide；
It is prepared by protection：98 parts of oxides, 50 parts of glacial acetic acid, 1500 parts of water, 40 parts of diazanyls are added in a kettle
Methyl formate, it is 20~25 DEG C to control temperature of reaction kettle, control reactor agitator shaft speed by 30-240r/min alternate transitions,
Wherein lowest speed continues 5 minutes every time, and most high speed continues 3 minutes every time, and after reacting 4-6 hours, centrifugal filtration obtains protection.
It is prepared by closed loop hydrolysate：120 parts of protection, 800 parts of chloroforms are added in a kettle, control reactor
Interior temperature is 25~28 DEG C, persistently stirs and is passed through ammonia, and control reactor agitator shaft speed is alternately turned by 30-300r/min
Become, wherein lowest speed continues 5 minutes every time, and most high speed continues 5 minutes every time, and reaction obtains intermediate after 10 hours；
940 parts of intermediates are pumped into washing kettle, after being washed with water once, are transferred in reactor, add 80 parts
Aceticanhydride, 100 parts of glacial acetic acid, control reactor agitator shaft speed are continued every time by 30-180r/min alternate transitions, wherein lowest speed
5 minutes, most high speed continued 1 minute every time, reacted 1 hour, after negative pressure is concentrated and dried, then added 1000 parts of first in a kettle
Alcohol, it is 0 DEG C to control reactor temperature, and 7.5 parts of boron hydrogen sodium are added in four times, and control reactor agitator shaft speed is by 20-
80r/min alternate transitions, wherein lowest speed continue 4 minutes every time, and most high speed continues 1 minute every time, after reacting 2-3 hours, add
Enter 10 parts of glacial acetic acid to neutralize, negative pressure concentration falls methanol, adds the ammonium hydrogen sulfate water that 1600 parts of mass percentage concentrations are 10%
Solution and 100 parts of formaldehyde, it is warming up to 40~45 DEG C and reacts 6 hours, then be down to 6 DEG C, centrifugal filtration, is washed to neutrality, dries
Crude product；
Above-mentioned crude product is put into decolouring kettle, 80 parts of dichloromethane is added, 500 parts of methanol dissolved clarifications, adds 5 parts of activity
Charcoal, decolourize 1 hour, be put into after filtering in concentration kettle, negative pressure concentration, freeze crystallization, centrifuge to obtain closed loop hydrolysate fine work；
Upper Iod R：75 parts of hydrolysate fine work are put into reactor, add 140 parts of methanol, 140 parts of dichloros
Methane, dissolved clarification is stirred, add 35 parts of calcium oxide, stir dissolved clarification at 25~30 DEG C, 70 parts of iodine are added dropwise in reactor, controlled
Reactor agitator shaft speed continues 3 minutes every time by 30-120r/min alternate transitions, wherein lowest speed, and most high speed continues 3 every time
Minute, control iodine, which is added dropwise, continues 1 hour, and it is that 20% glacial acetic acid solution carries out elutriation to add 420 parts of mass percentage concentrations, is centrifuged
Filter iodine thing；
Displacement reaction：125 parts of upper iodine things are put into reactor, add 700 parts of acetone, 84 parts of potassium acetates,
Lasting stirring, leads to nitrogen, is warming up to 56~58 DEG C, controls reactor agitator shaft speed by 30-180r/min alternate transitions, wherein
Lowest speed continues 5 minutes every time, and most high speed continues 1 minute every time, reacts 2 hours, and less than 50 DEG C concentration and recovery acetone of control are extremely
Distillated without acetone, add 1000 parts of water and carry out elutriation, be cooled to 20-25 DEG C, centrifuge dripping obtains semi-finished product；
The semi-finished product are put into decolouring kettle, 420 parts of methanol is added, 140 parts of dichloromethane dissolved clarifications, adds 7 parts of work
Property carbon decoloring, filter concentration, centrifugation, dry to obtain deflazacort finished product.
A kind of deflazacort fast reaction process example four：
Synthetic mesophase thing：3000g epoxies prednisolone and 120-150L organic solvents are added in a kettle, are passed through ammonia
Air is excluded, it is 25-45 DEG C to maintain temperature, after sustained response 20-30 hours, confirms that solution reaction is complete by thin-layered chromatography
Entirely, ammonia is removed, saturated aqueous common salt is added and washing 2-3 times is carried out to reactant, wash 1-2 times, reclaim organic solvent, then adopt
Recrystallized with decolourizing, obtain intermediate；
Reaction equation is：
It is prepared by crude product：3000g intermediates and 120-150L organic solvents are added in a kettle, add 3-6L aceticanhydrides,
100-200g acid catalysts, it is incubated in 25-45 DEG C, after continuing stirring reaction 12-18 hours, adds during ammoniacal liquor key section pH is
Property, cooling centrifugation elutriation obtains deflazacort crude product；
Reaction equation is：
Finished product crystallizes：Using crystallization kettle to above-mentioned crude product is carried out into decolouring crystallization, deflazacort finished product is obtained.
Wherein epoxy prednisolone can utilize androstenedione synthesis to be made.
Wherein organic solvent can be：Toluene, chloroform, dioxane, nitromethane.
Wherein acid catalyst can be：Hydrochloric acid, the sulfuric acid of inorganic acid, or the p-methyl benzenesulfonic acid of organic acid, trifluoroacetic acid.
Recrystallization decolourize using ethyl acetate, activated carbon.
The deflazacort prepared using this method can significantly reduce production cost, and production craft step is few, behaviour
Make simple and convenient.
It should be noted that herein, term " comprising ", "comprising" or its any other variant are intended to non-row
His property includes, so that process, method, article or equipment including a series of elements not only include those key elements, and
And also include the other element being not expressly set out, or also include for this process, method, article or equipment institute inherently
Key element.
Specific case used herein is set forth to the principle and embodiment of the present invention, the explanation of above example
It is only intended to help the method and its core concept for understanding the present invention.Described above is only the preferred embodiment of the present invention, should
When pointing out due to the finiteness of literal expression, and unlimited concrete structure objectively be present, for the common skill of the art
For art personnel, under the premise without departing from the principles of the invention, some improvement, retouching or change can also be made, can also incited somebody to action
Above-mentioned technical characteristic is combined by rights；These improve retouching, change or combination, or the not improved structure by invention
Think and technical scheme directly applies to other occasions, be regarded as protection scope of the present invention.
Claims (10)
1. a kind of quick production system of deflazacort, the reactor, elutriation kettle, centrifugal filtration that it includes being connected with each other according to process are set
Standby, concentration kettle, drying plant, decolouring kettle, the reactor include tank body (1), interlayer cavity (8) are provided with tank body (1) outer wall；
Characterized in that, it is evenly arranged with vertical temperature adjustment pipe (9) in the tank body (1)；It is provided centrally with stirring in the tank body (1)
Axle (2)；Agitating shaft (2) upper end connects magnetic couple rotating device (3) by static seal mode, and lower end is provided with paddle
Take turns (7)；Rotatable rotating cylinder (4) is provided with the agitating shaft (2)；Being provided with the rotating cylinder (4) oscilaltion and to revolve
The buoyancy impeller (6) turned；Buoyancy impeller (6) upper end is provided with can be with the lifting disk (5) that buoyancy impeller (6) move up and down；
The circular hole (51) for being socketed temperature adjustment pipe (9) is provided with the lifting disk (5)；Filter is evenly arranged with the lifting disk (5)
Water hole；Vertical chute (41) is evenly arranged with rotating cylinder (4) outer wall；On block set (64) inwall of the buoyancy impeller (6)
It is evenly arranged with the roller bearing (61) for coordinating with vertical chute (41)；Swivelling cover (71) upper end of the agitator arm (7) is equal
It is even to be provided with vertical upper keypad (72) in a ring；Rotating cylinder (4) lower end is provided with the lower keypad coordinated with upper keypad (72)
(42)。
A kind of 2. quick production system of deflazacort according to claim 1, it is characterised in that the agitator arm (7)
Including the blade (73) being uniformly arranged on swivelling cover (71)；The swivelling cover (71) is socketed on agitating shaft (2)；The rotation
Lid (71) inwall is evenly arranged with vertical interior keypad (74)；Agitating shaft (2) lower end is evenly arranged with and interior keypad (74)
The swinging plate (21) of cooperation.
3. the quick production system of a kind of deflazacort according to claim 2, it is characterised in that the swinging plate (21)
Highly it is less than the height of swivelling cover (71) inwall.
A kind of 4. quick production system of deflazacort according to claim 1, it is characterised in that block set (64) upper end
Face is uniformly inlaid with rotatable ball (62).
A kind of 5. quick production system of deflazacort according to claim 1, it is characterised in that block set (64) inwall
On be additionally provided with the arc scraper plate (63) moved in vertical chute (41).
6. the quick production system of a kind of deflazacort according to claim 1, it is characterised in that on the lifting disk (5)
Also it is evenly arranged with fixed impeller (52).
7. the quick production system of a kind of deflazacort according to claim 1, it is characterised in that in the temperature adjustment pipe (9)
It is provided with U-shaped conduit (93)；Heat filling (94) is provided between the U-shaped conduit (93) and temperature adjustment pipe (9)；It is described U-shaped to lead
Manage (93)；The temperature adjustment pipe (9) includes hot-water line (91) and condenser pipe (92)；The hot-water line (91) and condenser pipe (92) are mutual
It is arranged alternately.
A kind of 8. quick production system of deflazacort according to claim 1, it is characterised in that interlayer cavity (8) bag
Include the heating chamber (81) and cooling chamber (82) at interlaced interval.
9. a kind of deflazacort fast reaction technique according to claim any one of 1-8, it is characterised in that it is included such as
Lower preparation process：
It is prepared by oxide：Add in a kettle 80-120 part moulds dehydrogen substances, 150-250 parts glacial acetic acid, 20-50 parts chromic anhydride,
8-20 part manganese acetates, temperature is 35~38 DEG C in maintenance reaction kettle, and control reactor agitator shaft speed is replaced by 30-180r/min
Transformation, wherein lowest speed continues 5 minutes every time, and most high speed continues 2 minutes every time, after stirring reaction 2-3 hours, adds
After the sodium hydroxide solution that 1500-2000 parts mass percentage concentration is 5.4% carries out elutriation, centrifugal filtration obtains oxide；
Reaction equation is：
It is prepared by protection：In a kettle add 80-100 parts oxide, 30-70 parts glacial acetic acid, 1200-2000 parts water,
20-60 part methyl hydrazinocarboxylates, it is 20~25 DEG C to control temperature of reaction kettle, and control reactor agitator shaft speed is by 30-240r/
Min alternate transitions, wherein lowest speed continue 5 minutes every time, and most high speed continues 3 minutes every time, after reacting 4-6 hours, centrifuge
Filter to obtain protection；
Reaction equation is：
It is prepared by closed loop hydrolysate：100-140 parts protection, 600-1000 part chloroforms, control are added in a kettle
Reactor temperature is 25~28 DEG C, persistently stirs and is passed through ammonia, and control reactor agitator shaft speed is handed over by 30-300r/min
For transformation, wherein lowest speed continues 5 minutes every time, and most high speed continues 5 minutes every time, and intermediate is obtained after reacting 8-12 hours；
800-1000 parts intermediate is pumped into washing kettle, after being washed with water once, is transferred in reactor, adds 60-
100 parts of aceticanhydrides, 80-120 part glacial acetic acid, control reactor agitator shaft speed is by 30-180r/min alternate transitions, wherein lowest speed
Continue 5 minutes every time, most high speed continues 1 minute every time, reacts 0.8-1 hours, after negative pressure is concentrated and dried, then adds in a kettle
Enter 900-1200 part methanol, control reactor temperature as in ± 1 DEG C, 6-9 part boron hydrogen sodium is added in four times, control reactor
Agitator shaft speed continues 4 minutes every time by 20-80r/min alternate transitions, wherein lowest speed, and most high speed continues 1 minute every time, instead
Answer 2-3 hours, add 8-12 parts glacial acetic acid and neutralize, negative pressure concentration falls methanol, adds 1500-1800 part mass percentage concentrations
The ammonium hydrogen sulfate aqueous solution and 80-120 part formaldehyde for 10%, 40~45 DEG C of reaction 5-7 hours are warming up to, then are down to 5~10 DEG C,
Centrifugal filtration, neutrality is washed to, dries to obtain crude product；
Above-mentioned crude product is put into decolouring kettle, 60-90 part dichloromethane is added, 400-600 part methanol dissolved clarifications, adds 4-6 parts
Activated carbon, decolouring 0.5-1.5 hours, it is put into after filtering in concentration kettle, negative pressure concentration, freezes crystallization, centrifuge to obtain closed loop
Hydrolysate fine work；
Reaction equation is：
Upper Iod R：75 parts of hydrolysate fine work are put into reactor, add 120-160 part methanol, 120-160 parts
Dichloromethane, dissolved clarification is stirred, add 20-45 part calcium oxide, stir dissolved clarification at 25~30 DEG C, 50-80 part iodine is added dropwise to instead
Answer in kettle, control iodine, which is added dropwise, continues 0.8-1.2 hours, control reactor agitator shaft speed by 30-120r/min alternate transitions, its
Middle lowest speed continues 3 minutes every time, and most high speed continues 3 minutes every time；It is that 20% glacial acetic acid solution enters to add mass percentage concentration
Water-filling is analysed, and centrifugal filtration must go up iodine thing；
Reaction equation is：
Displacement reaction：Described 125 parts upper iodine things are put into reactor, 600-800 part acetone is added, adds 70-90 parts
Potassium acetate, lasting stirring, leads to nitrogen, is warming up to 56~58 DEG C, control reactor agitator shaft speed is alternately turned by 30-180r/min
Become, wherein lowest speed continues 5 minutes every time, and most high speed continues 1 minute every time, reacts 1.5-3 hours, controls less than 50 DEG C concentrations
Recovery acetone adds 900-1200 parts water and carries out elutriation, be cooled to 20-25 DEG C, centrifuge dripping obtains semi-finished product to being distillated without acetone；
The semi-finished product are put into decolouring kettle, 300-500 part methanol is added, 100-200 part dichloromethane dissolved clarifications, adds 5-
10 parts of activated carbon decolorizings, suction filtration are concentrated into small size, centrifuge, dry to obtain deflazacort finished product；
Reaction equation is：
10. a kind of deflazacort fast reaction technique according to claim 9, it is characterised in that it includes following prepare
Step：
It is prepared by oxide：100 parts of mould dehydrogen substances, 200 parts of glacial acetic acid, 40 parts of chromic anhydrides, 14 parts of manganese acetates are added in a kettle,
Temperature is 35~38 DEG C in maintenance reaction kettle, and control reactor agitator shaft speed is by 30-180r/min alternate transitions, wherein minimum
Speed continues 5 minutes every time, and most high speed continues 2 minutes every time, and after stirring reaction 2-3 hours, it is dense to add 1650 parts of quality percentages
After the sodium hydroxide solution spent for 5.4% carries out elutriation, centrifugal filtration obtains oxide；
It is prepared by protection：98 parts of oxides, 50 parts of glacial acetic acid, 1500 parts of water, 40 parts of carbazic acids are added in a kettle
Methyl esters, it is 20~25 DEG C to control temperature of reaction kettle, controls reactor agitator shaft speed by 30-240r/min alternate transitions, wherein
Lowest speed continues 5 minutes every time, and most high speed continues 3 minutes every time, and after reacting 4-6 hours, centrifugal filtration obtains protection.
It is prepared by closed loop hydrolysate：120 parts of protection, 800 parts of chloroforms are added in a kettle, control temperature in reactor
Spend for 25~28 DEG C, persistently stir and be passed through ammonia, control reactor agitator shaft speed by 30-300r/min alternate transitions, its
Middle lowest speed continues 5 minutes every time, and most high speed continues 5 minutes every time, and reaction obtains intermediate after 10 hours；
940 parts of intermediates are pumped into washing kettle, after being washed with water once, are transferred in reactor, add 80 parts of aceticanhydrides,
100 parts of glacial acetic acid, control reactor agitator shaft speed continue 5 points every time by 30-180r/min alternate transitions, wherein lowest speed
Clock, most high speed continue 1 minute every time, react 1 hour, after negative pressure is concentrated and dried, then add 1000 parts of methanol in a kettle, control
Reactor temperature processed is 0 DEG C, and 7.5 parts of boron hydrogen sodium are added in four times, and control reactor agitator shaft speed is by 20-80r/min
Alternate transition, wherein lowest speed continue 4 minutes every time, and most high speed continues 1 minute every time, after reacting 2-3 hours, add 10 parts of ice
Acetic acid neutralizes, and negative pressure concentration falls methanol, adds the ammonium hydrogen sulfate aqueous solution and 100 that 1600 parts of mass percentage concentrations are 10%
Part formaldehyde, it is warming up to 40~45 DEG C and reacts 6 hours, then be down to 6 DEG C, centrifugal filtration, is washed to neutrality, dries to obtain crude product；
Above-mentioned crude product is put into decolouring kettle, 80 parts of dichloromethane is added, 500 parts of methanol dissolved clarifications, adds 5 parts of activated carbons, take off
Color 1 hour, is put into concentration kettle after filtering, negative pressure concentration, freezes crystallization, centrifuges to obtain closed loop hydrolysate fine work；
Upper Iod R：75 parts of hydrolysate fine work are put into reactor, add 140 parts of methanol, 140 parts of dichloromethanes
Alkane, dissolved clarification is stirred, add 35 parts of calcium oxide, stir dissolved clarification at 25~30 DEG C, 70 parts of iodine are added dropwise in reactor, control is anti-
Kettle agitator shaft speed is answered to continue 3 minutes every time by 30-120r/min alternate transitions, wherein lowest speed, most high speed continues 3 points every time
Clock, control iodine, which is added dropwise, continues 1 hour, and it is that 20% glacial acetic acid solution carries out elutriation, centrifugal filtration to add 420 parts of mass percentage concentrations
Iodine thing must be gone up；
Displacement reaction：125 parts of upper iodine things are put into reactor, 700 parts of acetone is added, 84 parts of potassium acetates, continues
Stirring, lead to nitrogen, be warming up to 56~58 DEG C, control reactor agitator shaft speed is by 30-180r/min alternate transitions, wherein minimum
Speed continues 5 minutes every time, and most high speed continues 1 minute every time, reacts 2 hours, controls less than 50 DEG C concentration and recovery acetone to without third
Ketone distillates, and adds 1000 parts of water and carries out elutriation, is cooled to 20-25 DEG C, centrifuge dripping obtains semi-finished product；
The semi-finished product are put into decolouring kettle, 420 parts of methanol is added, 140 parts of dichloromethane dissolved clarifications, adds 7 parts of activated carbons
Decolourize, filter concentration, centrifugation, dry to obtain deflazacort finished product.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108484714A (en) * | 2018-03-13 | 2018-09-04 | 岳阳环宇药业有限公司 | The preparation process of deflazacort |
| CN117586335A (en) * | 2023-11-27 | 2024-02-23 | 湖南玉新药业有限公司 | Method for removing characteristic genotoxic impurities in deflazacort bulk drug |
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| CN103059096A (en) * | 2013-01-14 | 2013-04-24 | 仙居县圃瑞药业有限公司 | Synthesis method of deflazacort intermediate with [17a,16a-d] oxazoline structure |
| CN105777852A (en) * | 2014-12-22 | 2016-07-20 | 康普药业股份有限公司 | Deflazacort synthetic method |
| CN205413016U (en) * | 2016-03-17 | 2016-08-03 | 浙江圃瑞药业有限公司 | 17 reation kettle is used in alpha - hydroxyl progesterone production |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2932639A (en) * | 1955-02-02 | 1960-04-12 | Schering Corp | Delta1, 4-16, 17-oxido-pregnadienes |
| CN102936274A (en) * | 2012-11-12 | 2013-02-20 | 浙江仙居君业药业有限公司 | Preparation method for [17alpha, 16alpha-d] methyl oxazoline |
| CN103059096A (en) * | 2013-01-14 | 2013-04-24 | 仙居县圃瑞药业有限公司 | Synthesis method of deflazacort intermediate with [17a,16a-d] oxazoline structure |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108484714A (en) * | 2018-03-13 | 2018-09-04 | 岳阳环宇药业有限公司 | The preparation process of deflazacort |
| CN117586335A (en) * | 2023-11-27 | 2024-02-23 | 湖南玉新药业有限公司 | Method for removing characteristic genotoxic impurities in deflazacort bulk drug |
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