CN106000220A - Preparation method and application of organic solvent disintegrating tablet containing chemical reagent - Google Patents
Preparation method and application of organic solvent disintegrating tablet containing chemical reagent Download PDFInfo
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- CN106000220A CN106000220A CN201610505107.0A CN201610505107A CN106000220A CN 106000220 A CN106000220 A CN 106000220A CN 201610505107 A CN201610505107 A CN 201610505107A CN 106000220 A CN106000220 A CN 106000220A
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- 239000003960 organic solvent Substances 0.000 title claims abstract description 39
- 239000003153 chemical reaction reagent Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000000843 powder Substances 0.000 claims abstract description 74
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 30
- 238000006243 chemical reaction Methods 0.000 claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000000203 mixture Substances 0.000 claims abstract description 12
- 239000000853 adhesive Substances 0.000 claims abstract description 11
- 230000001070 adhesive effect Effects 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 10
- 238000000576 coating method Methods 0.000 claims description 24
- 239000011248 coating agent Substances 0.000 claims description 23
- 239000001993 wax Substances 0.000 claims description 17
- 239000004793 Polystyrene Substances 0.000 claims description 14
- 239000000463 material Substances 0.000 claims description 13
- 229920002223 polystyrene Polymers 0.000 claims description 12
- 239000012752 auxiliary agent Substances 0.000 claims description 9
- 239000004744 fabric Substances 0.000 claims description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000000428 dust Substances 0.000 claims description 5
- 239000011521 glass Substances 0.000 claims description 5
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 5
- 239000011707 mineral Substances 0.000 claims description 5
- 230000004907 flux Effects 0.000 claims description 4
- 229930195733 hydrocarbon Natural products 0.000 claims description 4
- 150000002430 hydrocarbons Chemical group 0.000 claims description 4
- 239000012184 mineral wax Substances 0.000 claims description 4
- 230000008859 change Effects 0.000 claims description 3
- 235000013312 flour Nutrition 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- 239000010409 thin film Substances 0.000 claims description 3
- 229920000642 polymer Polymers 0.000 claims description 2
- 238000005549 size reduction Methods 0.000 claims description 2
- 239000011230 binding agent Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 8
- 239000000126 substance Substances 0.000 abstract description 8
- 239000002699 waste material Substances 0.000 abstract description 6
- 239000007787 solid Substances 0.000 abstract description 5
- 230000008569 process Effects 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000005516 engineering process Methods 0.000 abstract description 2
- 231100000331 toxic Toxicity 0.000 abstract description 2
- 230000002588 toxic effect Effects 0.000 abstract description 2
- 238000003825 pressing Methods 0.000 abstract 1
- 238000007873 sieving Methods 0.000 abstract 1
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 17
- 239000002671 adjuvant Substances 0.000 description 16
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 12
- 239000004570 mortar (masonry) Substances 0.000 description 12
- RIOQSEWOXXDEQQ-UHFFFAOYSA-N triphenylphosphine Chemical compound C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 RIOQSEWOXXDEQQ-UHFFFAOYSA-N 0.000 description 12
- 239000012280 lithium aluminium hydride Substances 0.000 description 9
- UGOMMVLRQDMAQQ-UHFFFAOYSA-N xphos Chemical compound CC(C)C1=CC(C(C)C)=CC(C(C)C)=C1C1=CC=CC=C1P(C1CCCCC1)C1CCCCC1 UGOMMVLRQDMAQQ-UHFFFAOYSA-N 0.000 description 9
- 229910052763 palladium Inorganic materials 0.000 description 8
- 239000003814 drug Substances 0.000 description 7
- 238000006722 reduction reaction Methods 0.000 description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 235000013339 cereals Nutrition 0.000 description 6
- 230000009467 reduction Effects 0.000 description 6
- 239000011780 sodium chloride Substances 0.000 description 6
- 238000004132 cross linking Methods 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- 239000007800 oxidant agent Substances 0.000 description 4
- 230000001590 oxidative effect Effects 0.000 description 4
- 238000012216 screening Methods 0.000 description 4
- 238000006443 Buchwald-Hartwig cross coupling reaction Methods 0.000 description 3
- 229910010084 LiAlH4 Inorganic materials 0.000 description 3
- 239000012298 atmosphere Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 101100189356 Mus musculus Papolb gene Proteins 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 229910052927 chalcanthite Inorganic materials 0.000 description 2
- 239000003638 chemical reducing agent Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000002808 molecular sieve Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- QRUBYZBWAOOHSV-UHFFFAOYSA-M silver trifluoromethanesulfonate Chemical compound [Ag+].[O-]S(=O)(=O)C(F)(F)F QRUBYZBWAOOHSV-UHFFFAOYSA-M 0.000 description 2
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 1
- 229910001148 Al-Li alloy Inorganic materials 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000006069 Suzuki reaction reaction Methods 0.000 description 1
- JFBZPFYRPYOZCQ-UHFFFAOYSA-N [Li].[Al] Chemical compound [Li].[Al] JFBZPFYRPYOZCQ-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229960000583 acetic acid Drugs 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 229920005601 base polymer Polymers 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007907 direct compression Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- -1 part Substances 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 229950000845 politef Drugs 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000012429 reaction media Substances 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
- B01J2/006—Coating of the granules without description of the process or the device by which the granules are obtained
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B6/00—Hydrides of metals including fully or partially hydrided metals, alloys or intermetallic compounds ; Compounds containing at least one metal-hydrogen bond, e.g. (GeH3)2S, SiH GeH; Monoborane or diborane; Addition complexes thereof
- C01B6/24—Hydrides containing at least two metals; Addition complexes thereof
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/04—Chlorides
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
- C07F9/02—Phosphorus compounds
- C07F9/28—Phosphorus compounds with one or more P—C bonds
- C07F9/50—Organo-phosphines
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Molecular Biology (AREA)
- Medicinal Preparation (AREA)
Abstract
The invention relates to a preparation method and application of an organic solvent disintegrating tablet containing a chemical reagent. The preparation method is characterized by comprising the following steps: according to mass fractions, grinding 0.01-95% of target reagent powder, 0.1-99% of an adhesive, 0.1-50wt% of a disintegrating agent and 0-99% of other aid agents into fine powder; sieving the fine powder with a 100-mesh sieve, and then uniformly mixing the fine powder by use of a mixing machine; finally pressing the obtained tabletting mixture powder into tablets by use of a tabletting machine. The preparation method has the beneficial effects that chemicals are pressed into the tablets, so that the chemicals are convenient to use, accurate in dosage and convenient to convey, and contact between the chemicals and toxic reagents is less; chemical reagents sensitive to air and water can be protected; the feeding process can be simplified, and wastes are reduced; high-throughput chemical reaction in which solids are participated can be realized by virtue of the tabletting technology.
Description
Technical field
The present invention relates to preparation method and the application of a kind of organic solvent disintegrating tablet (O-Tab) containing chemical reagent.
Background technology
Synthetic Organic Chemistry is widely used in each neck such as medicine, pesticide, material, atomic energy, Aero-Space
Territory.But Synthetic Organic Chemistry is still one at present quite dangerous, labor-intensive industry.Organic conjunction
There is a lot of problem in the routine operation become: 1) Solid-state Chemistry medicine weighs time and effort consuming when using one by one；2) behaviour
Make contact during toxicity big chemical reagent pulverulence dangerous big；3) sensitive chemical reagent runs into water, air
Can react and cause danger；4) sensitive chemical reagent is rotten causes waste；5) glove box operation inconvenience is used；6)
Low dose of catalyst weighs inaccurate.
Modern medicines preparation technique is more ripe through semicentennial development, and wherein tablet takies the heaviest
The status wanted, direct compression of full-powder, production linkageization, the development of automatic high-speed high yield tablet machine is to improvement
The working condition of tablet and improve the quality of tablet and play huge impetus, be also simultaneously realize the present invention can
The premise of row.But most chemical reagent used in chemosynthesis will have more instead than clinical medicine
Ying Xing, so, it would be desirable to find high inert adjuvant.Such as adhesive and disintegrating agent, substantially can only adopt
With the most inert hydro carbons or the compound of fluorohydrocarbon class.And in order to not disturb GC or LC to analyze and after reaction
Process, adjuvant preferably insoluble in any solvent, so reaction terminate rear adjuvant can by simple filtration or
Centrifugal separator separates.
Nearest statistical data shows, Suzuki coupling reaction, Buchwald-Hartwig aminating reaction, use
Oxidation or the reduction reaction of making functional group conversions are the most frequently used several response types, and urging needed for these reactions
Agent, oxidant, reducing agent etc. often have fixing combination.Fixed Combination is pre-mixed by we, is prepared as
For tablet, it is possible to realize arranging reaction quickly and easily.
The screening of high flux reaction condition is the form with micro-reaction, performs to test with automation operating system
Journey, gathers experimental result data with sensitive quick detecting instrument, is analyzed locating to experimental data with computer
Managing, a large amount of samples are detected, thus reach the purpose of screening experiment optimum condition by the same time.Due to medicine
The screening of thing high flux reaction condition requires to process a large amount of sample simultaneously, the necessary milligram ammonia of experimental system, fluid sample
Can be measured by micropipette rifle etc., and the microweigh of the solid sample in organic solvent can not be substantially soluble in
But there is no relatively accurate method.
Summary of the invention
It is an object of the invention to: realize the conveniently, safely use of solid chemicals, and multicomponent chemical is tried
Mix reagent sheet is made in agent, applies in type reaction, reaches convenient, fast, the effect of little waste.
In order to achieve the above object, the technical scheme is that and provide a kind of organic solvent containing chemical reagent
The preparation method of disintegrating tablet, it is characterised in that comprise the following steps:
With size reduction machinery by mass fraction be 0.01～95% destination agent powder, 0.1%～99% adhesive,
0.1～the disintegrating agent of 50% and 0～99% other auxiliary agents wear into fine powder, fine powder is crossed and utilizes after the screen cloth of 100 mesh
Fine powder is fully mixed by mixing machinery, finally the press sheet mixture powder tablet machine obtained is pressed into tablet.
Preferably, other auxiliary agents described are mineral powder.
Preferably, described mineral powder is glass dust or silica flour.
Preferably, described adhesive is hydro carbons or fluorohydrocarbon polymer powder.
Preferably, described disintegrating agent is crosslinked polystyrene powder or rubber powder.
Preferably, described destination agent powder is single agents powder, or is the mixing of chemical reaction powder.
Preferably, it is coated described tablet to increase air and the stability of water.
Preferably, described coating is pressed coated, and the step increasing pressed coated outside described tablet includes:
In plunger die for tabletting press, it is previously added a part of coating material, then described tablet is placed on as label
Punch die middle, is eventually adding another part coating material, is pressed into coated tablet, and coating material is by described glutinous
The adhesive that mixture, described disintegrating agent and other auxiliary agents described mix.
Preferably, described coating is molten wax coating, and the step increasing molten wax coating outside described tablet includes:
Solidify after organic solvent disintegrating tablet being infiltrated with the mineral wax melted, form thin film, thus realize bag
Clothing.
Present invention also offers a kind of organic solvent disintegrating tablet prepared by above-mentioned preparation method should
With, it is characterised in that for high-throughout organic chemical reactions, with realize low dose, high flux, quick,
Can automation mechanized operation.
The invention has the beneficial effects as follows: 1) chemical drugs tabletted makes medicine easy to use, and consumption is accurate,
Convenient transportation, and can reduce and the contacting of toxic reagent；2) permissible to the chemical reagent of air, water sensitive
Protected, prevent from going bad, cause waste, removed from the loaded down with trivial details of glove box operation；3) mix reagent sheet is used
In common type reaction, the process that feeds intake can be simplified, and reduce waste；4) pressed-disc technique has made solid participate in
High throughput chemical reactions be possibly realized.
Accompanying drawing explanation
Fig. 1 (a) to Fig. 1 (d) is the example CuSO of the present invention4·5H2O sheet and LiAlH4Coated tablet is at water
Neutralize and stir comparison diagram in ethanol, wherein:
Fig. 1 (a) is CuSO4·5H2O sheet stirs in water；
Fig. 1 (b) is CuSO4·5H2O sheet stirs in ethanol；
Fig. 1 (c) is LiAlH4Coated tablet stirs in water；
Fig. 1 (d) is LiAlH4Coated tablet stirs in ethanol；
Fig. 2 (a) is CsF sheet water suction curves figure in atmosphere；
Fig. 2 (b) is NMO sheet water suction curves figure in atmosphere；
Fig. 2 (c) is AgOTf sheet water suction curves figure in atmosphere；
Fig. 3 is to be respectively adopted powder reagent and tablet carries out the kinetics of Buchwald-Hartwig aminating reaction
Comparison diagram.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is expanded on further.Should be understood that these embodiments are merely to illustrate
The present invention rather than restriction the scope of the present invention.In addition, it is to be understood that read the present invention lecture content it
After, the present invention can be made various changes or modifications by those skilled in the art, and these equivalent form of values fall within this equally
Application appended claims limited range.
The technical problem that present invention mainly solves is to provide the preparation side of a kind of organic solvent disintegrating tablet (O-Tab)
Method and coating method, it is achieved the conveniently, safely use of solid chemicals, and by multicomponent chemical reagent system
Become mix reagent sheet, apply in type reaction, reach convenient, fast, the effect of little waste, additionally will have
Machine solvent disintegrating tablet is applied to high-throughout organic chemical reactions, reaches the purpose of screening experiment condition.
The technical scheme is that and destination agent powder and the adjuvant such as adhesive, disintegrating agent are pressed into tablet.Contain
When the tablet of reagent contacts with reaction medium (usually organic solvent), disintegrating agent absorbs organic solvent, produces
Swelling, volumetric expansion causes the broken of whole tablet or disintegrate.Owing to our tablet can be in organic solvent
Fater disintegration, so we are called organic solvent disintegrating tablet.
Compacting organic solvent disintegrating tablet step is as follows: with mortar or ball mill, target chemical is worn into fine powder,
Destination agent and all of adjuvant cross the screen cloth of 100 mesh, and sieve removes bulky grain, with mortar or tube mill by chemistry
Product are sufficiently mixed with adjuvant, are pressed into tablet with tablet machine.
Wherein, the mass fraction of destination agent and all of adjuvant be 0.01～the destination agent powder of 95%,
The disintegrating agent of adhesive, 0.1～50% of 0.1%～99% and 0～other auxiliary agents of 99%.
Adhesive is hydro carbons or the fluorohydrocarbon base polymer powder such as politef (PTFE) wax micropowder, mineral wax powder
End.Disintegrating agent is crosslinked polystyrene powder, rubber powder etc..Other auxiliary agents (filler etc.) are glass dust,
Silica flour or other mineral powders.Destination agent can be single agents, it is also possible to be chemical reaction reagent (oxidation
Agent, reducing agent, catalyst, part, additive etc.) mixing.
For sensitive agents, organic solvent disintegrating tablet can be coated to increase air and the stability of water.Can
To be coated by compression coating.Coating steps is as follows: be previously added part bag in plunger die for tabletting press
Clothing material, is then placed on punch die middle using organic solvent disintegrating tablet as label, is eventually adding another part
Coating material, is pressed into coated tablet.Coating material is the mixture of adhesive, disintegrating agent and other auxiliary agents.
Can also be coated by molten wax method, coating steps is as follows: collapsed by organic solvent with the mineral wax melted
Solidify after solving sheet infiltration, form thin film, thus realize coating.
Organic solvent disintegrating tablet stability after coating is greatly increased, such as several organic containing strong absorptive reagent
Solvent disintegrating tablet water absorption is substantially reduced (see Fig. 2 (a) to Fig. 2 (c), CsF, NMO and AgOTf sheet
Aerial water suction curves).
Embodiment 1.NaCl organic solvent disintegrating tablet.
The NaCl organic solvent disintegrating tablet of the present embodiment, every includes the following raw material according to mass fraction meter:
NaCl powder (180.0mg, 83.3%), polytetrafluoroethylwax wax micropowder (34.3mg, 15.9%), crosslinking is poly-
Styrene powder (1.7mg, 0.8%).
The preparation method of the present embodiment, comprises the steps: to be worn into by sodium chloride crystal with mortar or ball mill
Fine powder, by above sodium chloride powder and all of adjuvant (polytetrafluoroethylwax wax micropowder, crosslinked polystyrene) mistake
The screen cloth of 100 mesh, sieve removes bulky grain, then with mortar or tube mill, sodium chloride powder is the most abundant with adjuvant
Mixing, is pressed into the sheet of a diameter of 6mm with tablet machine by above powder, and every tablet quality is 216.0mg.
Embodiment 2. triphenylphosphine organic solvent disintegrating tablet.
The triphenylphosphine organic solvent disintegrating tablet of the present embodiment, every include according to mass fraction meter the most former
Material: triphenylphosphine powder (70.0mg, 50.0%), polytetrafluoroethylwax wax micropowder (46.7mg, 33.4%),
Crosslinked polystyrene powder (2.3mg, 1.6%), glass dust (21.0mg, 15.0%).
The preparation method of the present embodiment, comprises the steps: to be ground by triphenylphosphine crystal with mortar or ball mill
Become fine powder, by above triphenylphosphine powder and all of adjuvant (polytetrafluoroethylwax wax micropowder, crosslinked polystyrene,
Glass dust) cross the screen cloth of 100 mesh, sieve removes bulky grain, then with mortar or tube mill by triphenylphosphine powder with auxiliary
Material is sufficiently mixed in proportion, above powder tablet machine is pressed into the sheet of a diameter of 6mm with tablet machine, often
Tablet quality is 140.0mg.
The preparation of embodiment 3. lithium aluminium hydride reduction organic solvent disintegrating tablet and coating.
The lithium aluminium hydride reduction organic solvent disintegrating tablet every of the present embodiment includes the following raw material according to mass fraction meter:
Lithium aluminium hydride reduction powder (19.0mg, 76.0%), polytetrafluoroethylwax wax micropowder (5.0mg, 20.0%), crosslinking
Polystyrene powder (1.0mg, 4.0%).
The preparation method of the present embodiment, comprises the steps: in glove box, with mortar or ball mill by hydrogen
Change aluminum lithium and wear into fine powder, by above lithium aluminium hydride reduction powder and all of adjuvant (polytetrafluoroethylwax wax micropowder, crosslinking
Polystyrene) cross the screen cloth of 100 mesh, sieve removes bulky grain, then with mortar or tube mill by lithium aluminium hydride reduction powder with
Adjuvant is sufficiently mixed in proportion, and above powder tablet machine is pressed into the sheet of a diameter of 4mm with tablet machine,
Every tablet quality is 25.0mg.With the coating material of ratio as adjuvant, lithium aluminium hydride reduction label is coated again,
A diameter of 6mm of coated tablet, tablet weight 120mg.
Embodiment 4. palladium and part (XPhos) organic solvent disintegrating tablet are applied to Buchwald-Hartwig amine
Change reaction
The palladium organic solvent disintegrating tablet of the present embodiment, every includes the following raw material according to mass fraction meter:
Palladium powder (2.24mg, 22.4%), polytetrafluoroethylwax wax micropowder (7.39mg, 73.9%), crosslinking is poly-
Styrene powder (0.37mg, 3.7%).The XPhos organic solvent disintegrating tablet of the present embodiment, every include by
Following raw material according to mass fraction meter: XPhos powder (4.76mg, 47.6%), polytetrafluoroethylwax wax micropowder
(4.99mg, 49.9%), crosslinked polystyrene powder (0.25mg, 2.50%).
The preparation method of the present embodiment, comprises the steps: in glove box, with mortar or ball mill by vinegar
Acid palladium and XPhos wear into fine powder, and by above palladium, XPhos and all of adjuvant, (polytetrafluoroethylwax wax is micro-
Powder, crosslinked polystyrene) cross the screen cloth of 100 mesh, sieve removes bulky grain, then with mortar or tube mill by palladium
Or XPhos is sufficiently mixed with adjuvant in proportion, with tablet machine, above powder tablet machine is pressed into diameter equal
Palladium sheet and XPhos sheet for 4mm.
Following reaction is carried out respectively with palladium, XPhos powder and the palladium sheet being pressed into, XPhos sheet,
Kinetics comparison diagram is as shown in Figure 3.
Embodiment 5. oxidant mixed organic solvents disintegrating tablet (OX-tab).
The oxidant mixing tab of the present embodiment, every includes the following raw material according to mass fraction meter: four n-pro-pyls
Cross ruthenic acid ammonium (TPAP) powder (1.76mg, 2.1%), N-methyl-N-morpholine oxide (NMO) powder (17.60
Mg, 21.1%),Molecular sieve powder (50.00mg, 60.1%), polytetrafluoroethylwax wax micropowder (13.20mg,
15.9%), crosslinked polystyrene powder (0.66mg, 0.8%).
The preparation method of the present embodiment, comprises the steps: TPAP, NMO with mortar or ball mill,Fine powder worn into respectively by molecular sieve, by above fine powder and all of adjuvant (polytetrafluoroethylwax wax micropowder, crosslinking
Polystyrene) cross the screen cloth of 100 mesh, sieve removes bulky grain, then with mortar or tube mill by all powder in proportion
It is sufficiently mixed, with tablet machine, above powder tablet machine is pressed into diameter and is the mix reagent sheet of 6mm,
Every tablet quality 83.2mg.
Carry out following oxidation reaction with prepared oxidant mixing tab, obtain the conversion ratio of 99%.
Claims (10)
1. the preparation method of the organic solvent disintegrating tablet containing chemical reagent, it is characterised in that comprise the following steps:
With size reduction machinery by mass fraction be 0.01～95% destination agent powder, 0.1%～99% adhesive,
0.1～the disintegrating agent of 50% and 0～99% other auxiliary agents wear into fine powder, utilize mixing machinery after fine powder is crossed screen cloth
Fine powder is fully mixed, finally the press sheet mixture powder tablet machine obtained is pressed into tablet.
A kind of preparation method of the organic solvent disintegrating tablet containing chemical reagent, its feature
Being, other auxiliary agents described are mineral powder.
A kind of preparation method of the organic solvent disintegrating tablet containing chemical reagent, its feature
Being, described mineral powder is glass dust or silica flour.
A kind of preparation method of the organic solvent disintegrating tablet containing chemical reagent, its feature
Being, described adhesive is hydro carbons or fluorohydrocarbon polymer powder.
A kind of preparation method of the organic solvent disintegrating tablet containing chemical reagent, its feature
Being, described disintegrating agent is crosslinked polystyrene powder or rubber powder.
A kind of preparation method of the organic solvent disintegrating tablet containing chemical reagent, its feature
Being, described destination agent powder is single agents powder, or is the mixing of chemical reaction powder.
A kind of preparation method of the organic solvent disintegrating tablet containing chemical reagent, its feature
It is, is coated described tablet to increase air and the stability of water.
A kind of preparation method of the organic solvent disintegrating tablet containing chemical reagent, its feature
Being, described coating is pressed coated, and the step increasing pressed coated outside described tablet includes:
In plunger die for tabletting press, it is previously added a part of coating material, then described tablet is placed on as label
Punch die middle, is eventually adding another part coating material, is pressed into coated tablet, and coating material is by described glutinous
The binding agent that mixture, described disintegrating agent and other auxiliary agents described mix.
A kind of preparation method of the organic solvent disintegrating tablet containing chemical reagent, its feature
Being, described coating is molten wax coating, and the step increasing molten wax coating outside described tablet includes:
Solidify after organic solvent disintegrating tablet being infiltrated with the mineral wax melted, form thin film, thus realize bag
Clothing.
10. an application for the organic solvent disintegrating tablet prepared by the preparation method described in claim 1, its
Be characterised by, for high-throughout organic chemical reactions, with realize low dose, high flux, quick, can be automatic
Change operation.
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| CN201610505107.0A CN106000220A (en) | 2016-06-30 | 2016-06-30 | Preparation method and application of organic solvent disintegrating tablet containing chemical reagent |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610505107.0A CN106000220A (en) | 2016-06-30 | 2016-06-30 | Preparation method and application of organic solvent disintegrating tablet containing chemical reagent |
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| CN106000220A true CN106000220A (en) | 2016-10-12 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107638883A (en) * | 2017-09-28 | 2018-01-30 | 江苏迈川工程技术研究院有限公司 | Catalyst, preparation and application for the direct synthesizing low-carbon alkene of F- T synthesis |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1429133A (en) * | 2000-03-17 | 2003-07-09 | H·隆德贝克有限公司 | Dosing form for reagents, use of said dosing form in organic chemical synthesis and production of said dosing form |
| CN105007899A (en) * | 2012-12-20 | 2015-10-28 | 卡希夫制药有限责任公司 | Orally disintegrating tablet formulation for enhanced bioavailability |
| CN105708819A (en) * | 2011-11-23 | 2016-06-29 | 诺华股份有限公司 | Pharmaceutical formulations |
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2016
- 2016-06-30 CN CN201610505107.0A patent/CN106000220A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1429133A (en) * | 2000-03-17 | 2003-07-09 | H·隆德贝克有限公司 | Dosing form for reagents, use of said dosing form in organic chemical synthesis and production of said dosing form |
| CN105708819A (en) * | 2011-11-23 | 2016-06-29 | 诺华股份有限公司 | Pharmaceutical formulations |
| CN105007899A (en) * | 2012-12-20 | 2015-10-28 | 卡希夫制药有限责任公司 | Orally disintegrating tablet formulation for enhanced bioavailability |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107638883A (en) * | 2017-09-28 | 2018-01-30 | 江苏迈川工程技术研究院有限公司 | Catalyst, preparation and application for the direct synthesizing low-carbon alkene of F- T synthesis |
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