CN107383053B - A kind of purification process of moxidectin crude product - Google Patents
A kind of purification process of moxidectin crude product Download PDFInfo
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- CN107383053B CN107383053B CN201710609366.2A CN201710609366A CN107383053B CN 107383053 B CN107383053 B CN 107383053B CN 201710609366 A CN201710609366 A CN 201710609366A CN 107383053 B CN107383053 B CN 107383053B
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- moxidectin
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- YZBLFMPOMVTDJY-CBYMMZEQSA-N moxidectin Chemical compound O1[C@H](C(\C)=C\C(C)C)[C@@H](C)C(=N/OC)\C[C@@]11O[C@H](C\C=C(C)\C[C@@H](C)\C=C\C=C/2[C@]3([C@H](C(=O)O4)C=C(C)[C@@H](O)[C@H]3OC\2)O)C[C@H]4C1 YZBLFMPOMVTDJY-CBYMMZEQSA-N 0.000 title claims abstract description 75
- 229960004816 moxidectin Drugs 0.000 title claims abstract description 75
- 239000012043 crude product Substances 0.000 title claims abstract description 27
- 238000000746 purification Methods 0.000 title claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 29
- 239000011347 resin Substances 0.000 claims abstract description 16
- 229920005989 resin Polymers 0.000 claims abstract description 16
- 238000001179 sorption measurement Methods 0.000 claims abstract description 14
- 238000004090 dissolution Methods 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 40
- 239000008213 purified water Substances 0.000 claims description 32
- 239000000243 solution Substances 0.000 claims description 25
- 238000001914 filtration Methods 0.000 claims description 19
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 18
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 claims description 17
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 claims description 17
- 238000003756 stirring Methods 0.000 claims description 17
- 238000001035 drying Methods 0.000 claims description 15
- 239000003463 adsorbent Substances 0.000 claims description 11
- 238000010521 absorption reaction Methods 0.000 claims description 9
- 239000004411 aluminium Substances 0.000 claims description 9
- 229910052782 aluminium Inorganic materials 0.000 claims description 9
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 9
- 239000013078 crystal Substances 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 7
- 238000010792 warming Methods 0.000 claims description 7
- 238000002425 crystallisation Methods 0.000 claims description 3
- 230000008025 crystallization Effects 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims 1
- 229960000583 acetic acid Drugs 0.000 claims 1
- DCKVNWZUADLDEH-UHFFFAOYSA-N sec-butyl acetate Chemical compound CCC(C)OC(C)=O DCKVNWZUADLDEH-UHFFFAOYSA-N 0.000 claims 1
- 239000000047 product Substances 0.000 abstract description 8
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 238000000605 extraction Methods 0.000 abstract description 5
- 239000012535 impurity Substances 0.000 abstract description 3
- 238000000855 fermentation Methods 0.000 description 5
- 230000004151 fermentation Effects 0.000 description 5
- 239000007787 solid Substances 0.000 description 5
- 230000003115 biocidal effect Effects 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 241001655322 Streptomycetales Species 0.000 description 2
- 230000000507 anthelmentic effect Effects 0.000 description 2
- 238000004587 chromatography analysis Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000001953 recrystallisation Methods 0.000 description 2
- 239000005660 Abamectin Substances 0.000 description 1
- GUBGYTABKSRVRQ-XLOQQCSPSA-N Alpha-Lactose Chemical compound O[C@@H]1[C@@H](O)[C@@H](O)[C@@H](CO)O[C@H]1O[C@@H]1[C@@H](CO)O[C@H](O)[C@H](O)[C@H]1O GUBGYTABKSRVRQ-XLOQQCSPSA-N 0.000 description 1
- 241000238421 Arthropoda Species 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- -1 Cyclic lactone Chemical class 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- 244000068988 Glycine max Species 0.000 description 1
- 235000010469 Glycine max Nutrition 0.000 description 1
- GUBGYTABKSRVRQ-QKKXKWKRSA-N Lactose Natural products OC[C@H]1O[C@@H](O[C@H]2[C@H](O)[C@@H](O)C(O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@H]1O GUBGYTABKSRVRQ-QKKXKWKRSA-N 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- HMSYAPGFKGSXAJ-PAHGNTJYSA-N Mocimycin Chemical compound C(/[C@H]1O[C@H]([C@H]([C@H]1O)O)[C@H](C)[C@H](OC)C(/C)=C/C=C/CNC(=O)[C@@H](CC)[C@]1(O)[C@@H]([C@H](O)C(C)(C)[C@H](\C=C\C=C/C)O1)O)=C\C=C\C=C(/C)C(=O)C1=C(O)NC=CC1=O HMSYAPGFKGSXAJ-PAHGNTJYSA-N 0.000 description 1
- 239000001888 Peptone Substances 0.000 description 1
- 108010080698 Peptones Proteins 0.000 description 1
- 235000014680 Saccharomyces cerevisiae Nutrition 0.000 description 1
- 240000004808 Saccharomyces cerevisiae Species 0.000 description 1
- 230000001679 anti-nematodal effect Effects 0.000 description 1
- 239000003096 antiparasitic agent Substances 0.000 description 1
- 229940125687 antiparasitic agent Drugs 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- RRZXIRBKKLTSOM-XPNPUAGNSA-N avermectin B1a Chemical compound C1=C[C@H](C)[C@@H]([C@@H](C)CC)O[C@]11O[C@H](C\C=C(C)\[C@@H](O[C@@H]2O[C@@H](C)[C@H](O[C@@H]3O[C@@H](C)[C@H](O)[C@@H](OC)C3)[C@@H](OC)C2)[C@@H](C)\C=C\C=C/2[C@]3([C@H](C(=O)O4)C=C(C)[C@@H](O)[C@H]3OC\2)O)C[C@H]4C1 RRZXIRBKKLTSOM-XPNPUAGNSA-N 0.000 description 1
- FFBHFFJDDLITSX-UHFFFAOYSA-N benzyl N-[2-hydroxy-4-(3-oxomorpholin-4-yl)phenyl]carbamate Chemical compound OC1=C(NC(=O)OCC2=CC=CC=C2)C=CC(=C1)N1CCOCC1=O FFBHFFJDDLITSX-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 235000012343 cottonseed oil Nutrition 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 125000002791 glucosyl group Chemical group C1([C@H](O)[C@@H](O)[C@H](O)[C@H](O1)CO)* 0.000 description 1
- 239000001963 growth medium Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 150000002596 lactones Chemical class 0.000 description 1
- 239000008101 lactose Substances 0.000 description 1
- 239000003120 macrolide antibiotic agent Substances 0.000 description 1
- 229940041033 macrolides Drugs 0.000 description 1
- 235000012054 meals Nutrition 0.000 description 1
- FXWHFKOXMBTCMP-WMEDONTMSA-N milbemycin Natural products COC1C2OCC3=C/C=C/C(C)CC(=CCC4CC(CC5(O4)OC(C)C(C)C(OC(=O)C(C)CC(C)C)C5O)OC(=O)C(C=C1C)C23O)C FXWHFKOXMBTCMP-WMEDONTMSA-N 0.000 description 1
- 229950008095 mocimycin Drugs 0.000 description 1
- HMSYAPGFKGSXAJ-KNHRXMRASA-N mocimycin Natural products C([C@H]1O[C@H]([C@H]([C@H]1O)O)[C@H](C)[C@H](OC)C(C)=CC=CCNC(=O)[C@@H](CC)[C@]1(O)[C@@H]([C@H](O)C(C)(C)[C@H](C=CC=CC)O1)O)=CC=CC=C(C)C(=O)C1=C(O)NC=CC1=O HMSYAPGFKGSXAJ-KNHRXMRASA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 244000045947 parasite Species 0.000 description 1
- 235000019319 peptone Nutrition 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D493/00—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system
- C07D493/22—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system in which the condensed system contains four or more hetero rings
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Heterocyclic Carbon Compounds Containing A Hetero Ring Having Oxygen Or Sulfur (AREA)
- Saccharide Compounds (AREA)
Abstract
The present invention relates to a kind of method of moxidectin purifying crude, processing steps are as follows: by moxidectin crude product through dissolution, resin adsorption, crystallize and be dried to obtain moxidectin sterling.The present invention carries out the extraction purification of moxidectin by the way of resin adsorption, the impurity in moxidectin is eliminated to greatest extent, effectively improve moxidectin finished product content, its finished product content has reached 97% or more, product quality meets European Pharmacopoeia quality standard, while present invention process is simple, with short production cycle, production cost is low, is conducive to improve moxidectin competitiveness in the international market.
Description
Technical field
The invention belongs to antibiotic extractive technique fields, more particularly to a kind of purification process of moxidectin crude product.
Background technique
Moxidectin (MXD) be a kind of wide spectrum for being now widely used in veterinary clinic, efficiently, Novel macrocyclic lactone expelling parasite
Antibiotic is a member in milbemycin family.MXD be by a kind of streptomycete fermentation generate, semi-synthetic single component it is big
Cyclic lactone class antibiotic, be how the derivative of horse rhzomorph.MXD and other macrolides antiparasitic agents and avermectin
The difference is that it is single component, there are higher anthelmintic activity and the characteristics such as long-acting, safe, and just have under very low dose
Epizoa is active in vivo for very strong anti-nematode and arthropod etc., and 20th century, the mid-80 was initially as anthelmintic for animals
It uses.
Currently, domestic open source literature sketched using ethyl alcohol extract how horse rhzomorph, by extraction, chromatography, decoloration, oxidation and
The methods of oximate obtains moxidectin crude product, then utilizes the method extraction purification moxidectin of recrystallization.Existing for this method
Problem is: cannot be effectively removed the impurity of moxidectin using the method for recrystallization, cause finished product effective content lower, do not surpass
Cross 94%.
Summary of the invention
It is an object of the invention to overcome above-mentioned defect in the prior art, establishing one kind, to effectively remove moxidectin miscellaneous
Matter improves the purification process of the moxidectin crude product of finished product content.
The technical solution taken to achieve the above object are as follows:
A kind of purification process of moxidectin crude product, it is characterised in that its processing step are as follows:
1) it dissolves
The mixed solution that aluminium polychloride, adsorbent and purified water that mocimycin crude product is 7.5-8.0 with pH are formed
Dissolution, is added butyl acetate after being sufficiently stirred, and continues to stir certain time, then filter, stand, layered filtration obtains Moses bacterium
Plain butyl acetate solution；
2) resin adsorption
It is molten that gained moxidectin butyl acetate solution is obtained into moxidectin after super high cross-linked adsorbing resin absorption, parsing
Liquid；
3) it crystallizes
Purified water is added in moxidectin solution, is warming up to 48-50 DEG C, continuously adds purified water, crystallization to appear is existing
As rear stopping addition purified water, is stood after being sufficiently stirred, moxidectin crystal is obtained by filtration；
4) dry.
The process 1) in, purifying water consumption is 11-15 times of moxidectin crude product quality；Aluminium polychloride dosage is not
The 3-5% of western rhzomorph crude product quality；Adsorbent amount is the 0.4-0.8% of moxidectin crude product quality；Butyl acetate dosage is not
7-9 times of western rhzomorph crude product quality.
The adsorbent selects novel heavy metal sewage treating material NSUL-2 adsorbent.
The process 2) in, super high cross-linked adsorbing resin absorption adsorbs resin using Ambeilite XAD-6, and dosage is
3-5 times of moxidectin crude product quality.
The method of describedization, it is characterised in that the process 2) in, in adsorption process, adsorption flow rate is controlled in 3-4L/
min。
The process 2) in, in resolving, desorbed solution is acetone, parses flow control in 5-6L/min.
The process 3) in, 3-5 times that purifying water consumption is acetone soln volume is added for the first time；It is pure in crystallization process
Change the flow control of water in 6-8L/min.
The process 4) in, it is dry to use double conic rotary vacuum dryer, 60~80 DEG C of drying temperature, vacuum degree is-
0.02~-0.08 MPa, 12~16h of drying time.
The present invention carries out the extraction purification of moxidectin by the way of resin adsorption, eliminates Moses bacterium to greatest extent
Impurity in element effectively improves moxidectin finished product content, and finished product content has reached 97% or more, and product quality meets Europe
Pharmacopoeial quality standard, while present invention process is simple, with short production cycle, production cost is low, is conducive to improve the moxidectin world
The market competitiveness.
Specific implementation method
The present invention will be described below by way of examples, it should be understood that example is for illustrating rather than to this
The limitation of invention.The scope of the present invention is determined with core content according to claims.
Fermentation liquid source in following embodiments:
Using second order fermentation mode of manufacture how horse rhzomorph, production strain be streptomycete, how horse rhzomorph culture medium carbon source is
Glucose, lactose；Nitrogen source soybean cake powder, cottonseed meal, peptone and yeast powder, cultivation temperature are 28 DEG C, and fermentation period is
240-280h, fermentation unit is generally in 2000-2500ug/ml.How horse rhzomorph passes through extraction, chromatography, decolourizes, oxygen the gained that will ferment
The methods of change and oximate obtain moxidectin crude product.
Embodiment 1
Moxidectin crude product 10kg is separately added into purified water 110L, aluminium polychloride H8150 0.3kg and adsorbent
NSUL-2 0.04kg adjusts pH to 7.5 with lye, stirs 20min.
Butyl acetate 70L is added, stirs 40min, filtering.
Mixed solution stands 60min, and then layered filtration obtains moxidectin butyl acetate solution 64.4L.
In adsorption process, the super high cross-linked adsorbing resin used is Ambeilite XAD-6, dosage 30kg, absorption
Flow control is in 3L/min.
In resolving, desorbed solution is acetone, and dosage 60.7L parses flow control in 5L/min.
Purified water 183L is added in moxidectin organic solution, and is warming up to 48 DEG C, continuously adds purified water, purified water
Flow control in 6L/min, after there is crystalline polamer stop that purified water is added, continue to stir 40min, be then allowed to stand 80min,
The wet crystal 12.3kg of moxidectin is obtained after filtering.
Dry to use double conic rotary vacuum dryer, 60~80 DEG C of drying temperature, vacuum degree is -0.02~-0.08 MPa,
Drying time 12h obtains moxidectin solid 8.9kg.
Through detecting, moxidectin effective content is 97.2%.
Embodiment 2
Moxidectin crude product 10kg is separately added into purified water 120L, aluminium polychloride H8150 0.35kg and adsorbent
NSUL-2 0.05kg adjusts pH to 7.6 with lye, stirs 23min.
Butyl acetate 75L is added, stirs 45min, filtering.
Mixed solution stands 65min, and then layered filtration obtains moxidectin butyl acetate solution 69L.
In adsorption process, the super high cross-linked adsorbing resin used is Ambeilite XAD-6, dosage 35kg, absorption
Flow control is in 3.2L/min.
In resolving, desorbed solution is acetone, and dosage 65.4L parses flow control in 5.2L/min.
Purified water 229L is added in moxidectin organic solution, and is warming up to 48.5 DEG C, continuously adds purified water, purifies
The flow control of water after there is crystalline polamer stops that purified water is added, continues to stir 45min, be then allowed to stand in 6.5L/min
85min obtains the wet crystal 12.2kg of moxidectin after filtering.
Dry to use double conic rotary vacuum dryer, 60~80 DEG C of drying temperature, vacuum degree is -0.02~-0.08 MPa,
Drying time 13h obtains moxidectin solid 8.8kg.
Through detecting, moxidectin effective content is 97.4%.
Embodiment 3
Moxidectin crude product 10kg is separately added into purified water 130L, aluminium polychloride H8150 0.4kg and adsorbent
NSUL-2 0.06kg adjusts pH to 7.7 with lye, stirs 25min.
Butyl acetate 80L is added, stirs 50min, filtering.
Mixed solution stands 70min, and then layered filtration obtains moxidectin butyl acetate solution 74L.
In adsorption process, the super high cross-linked adsorbing resin used is Ambeilite XAD-6, dosage 40kg, absorption
Flow control is in 3.5L/min.
In resolving, desorbed solution is acetone, and dosage 70L parses flow control in 5.5L/min.
Purified water 280L is added in moxidectin organic solution, and is warming up to 49 DEG C, continuously adds purified water, purified water
Flow control in 7L/min, after there is crystalline polamer stop that purified water is added, continue to stir 50min, be then allowed to stand 90min,
The wet crystal 12.4kg of moxidectin is obtained after filtering.
Dry to use double conic rotary vacuum dryer, 60~80 DEG C of drying temperature, vacuum degree is -0.02~-0.08 MPa,
Drying time 14h obtains moxidectin solid 8.9kg.
Through detecting, moxidectin effective content is 97.8%.
Embodiment 4
Moxidectin crude product 10kg is separately added into purified water 140L, aluminium polychloride H8150 0.45kg and adsorbent
NSUL-2 0.07kg adjusts pH to 7.9 with lye, stirs 28min.
Butyl acetate 85L is added, stirs 55min, filtering.
Mixed solution stands 75min, and then layered filtration obtains moxidectin butyl acetate solution 78L.
In adsorption process, the super high cross-linked adsorbing resin used is Ambeilite XAD-6, dosage 45kg, absorption
Flow control is in 3.7L/min.
In resolving, desorbed solution is acetone, and dosage 72L parses flow control in 5.8L/min.
Purified water 324L is added in moxidectin organic solution, and is warming up to 49.5 DEG C, continuously adds purified water, purifies
The flow control of water after there is crystalline polamer stops that purified water is added, continues to stir 55min, be then allowed to stand in 7.5L/min
95min obtains the wet crystal 12.3kg of moxidectin after filtering.
Dry to use double conic rotary vacuum dryer, 60~80 DEG C of drying temperature, vacuum degree is -0.02~-0.08 MPa,
Drying time 15h obtains moxidectin solid 8.8kg.
Through detecting, moxidectin effective content is 97.6%.
Embodiment 5
Moxidectin crude product 10kg is separately added into purified water 150L, aluminium polychloride H8150 0.5kg and adsorbent
NSUL-2 0.08kg adjusts pH to 8.0 with lye, stirs 30min.
Butyl acetate 90L is added, stirs 60min, filtering.
Mixed solution stands 80min, and then layered filtration obtains moxidectin butyl acetate solution 84L.
In adsorption process, the super high cross-linked adsorbing resin used is Ambeilite XAD-6, dosage 50kg, absorption
Flow control is in 4L/min.
In resolving, desorbed solution is acetone, and dosage 80L parses flow control in 6L/min.
Purified water 400L is added in moxidectin organic solution, and is warming up to 50 DEG C, continuously adds purified water, purified water
Flow control in 8L/min, after there is crystalline polamer stop that purified water is added, continue to stir 60min, be then allowed to stand 100min,
The wet crystal 12.1kg of moxidectin is obtained after filtering.
Dry to use double conic rotary vacuum dryer, 60~80 DEG C of drying temperature, vacuum degree is -0.02~-0.08 MPa,
Drying time 16h obtains moxidectin solid 8.7kg.
Through detecting, moxidectin effective content is 97.5%.
Claims (3)
1. a kind of purification process of moxidectin crude product, it is characterised in that its processing step are as follows:
1) it dissolves
The mixed solution dissolution that aluminium polychloride, adsorbent and purified water that moxidectin crude product is 7.5-8.0 with pH are formed,
Butyl acetate is added after being sufficiently stirred, continues to stir certain time, then filter, stand, layered filtration obtains moxidectin vinegar
Acid butyl ester solution；Wherein purifying water consumption is 11-15 times of moxidectin crude product quality；Aluminium polychloride dosage is moxidectin
The 3-5% of crude product quality；Adsorbent selects heavy metal-polluted water process material NSUL-2, and dosage is moxidectin crude product quality
0.4-0.8%；Butyl acetate dosage is 7-9 times of moxidectin crude product quality；
2) resin adsorption
Gained moxidectin butyl acetate solution is obtained after desorbed solution parsing through super high cross-linked adsorbing resin absorption, using acetone
Moxidectin solution, in above-mentioned adsorption process, adsorption flow rate is controlled in 3-4L/min, resolving, and parsing flow control exists
5-6L/m；The super high cross-linked adsorbing resin absorption adsorbs resin using Ambeilite XAD-6, and dosage is that moxidectin is thick
3-5 times of quality；
3) it crystallizes
Purified water is added in moxidectin solution, is warming up to 48-50 DEG C, continuously adds purified water, after crystalline polamer to appear
Stop that purified water is added, is stood after being sufficiently stirred, moxidectin crystal is obtained by filtration；
4) dry.
2. the purification process of moxidectin crude product described in accordance with the claim 1, it is characterised in that the process 3) in, for the first time
It is added 3-5 times that purifying water consumption is acetone soln volume；In crystallization process, the flow control of purified water is in 6-8L/min.
3. the purification process of moxidectin crude product described in accordance with the claim 1, it is characterised in that the process 4) in, drying is adopted
With double conic rotary vacuum dryer, 60~80 DEG C of drying temperature, vacuum degree is -0.02~-0.08 MPa, drying time 12~
16h。
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| CN104628740A (en) * | 2015-02-13 | 2015-05-20 | 河北圣雪大成制药有限责任公司 | Method for chemical synthesis and purification of moxidectin |
| CN105001232A (en) * | 2015-07-08 | 2015-10-28 | 安徽省皖北药业股份有限公司 | Purification method for moxidectin |
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2017
- 2017-07-25 CN CN201710609366.2A patent/CN107383053B/en active Active
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4916154A (en) * | 1986-09-12 | 1990-04-10 | American Cyanamid Company | 23-Imino derivatives of LL-F28249 compounds |
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