15 results about "Isopropyl acetate" patented technology

The invention discloses a preparation method of an abesilib III crystal form, which comprises the following steps of: 1, adding an abesilib crude product into DMSO (Dimethylsulfoxide), heating and dissolving, cooling after the system is dissolved to be clear, then adding isopropyl acetate, stirring, cooling and crystallizing, and then stirring, carrying out suction filtration and vacuum drying to obtain the abesilib III crystal form; or the method II comprises the following steps: adding the crude product of abelsilib into isopropyl acetate, stirring for crystal transformation, then cooling for crystallization, stirring, carrying out suction filtration, and carrying out vacuum drying to obtain the crystal form III of abelsilib. According to the preparation method, DMSO is adopted as a solvent, isopropyl acetate is adopted as a crystallization solvent, or isopropyl acetate is adopted as a crystal transformation solvent, the prepared abelsilib III crystal form is good in quality and high in yield, the process is simple, the requirement for equipment is low, the production period is short, the production cost is effectively reduced, and industrial mass production is easy to achieve.

The invention belongs to the technical field of cosmetics, and provides a preparation method of a piper nigrum root extract and application of the piper nigrum root extract in pain relieving cosmetics. The kava pepper root extract is prepared by the following steps: crushing kava pepper roots, and performing alcohol extraction; carrying out secondary extraction by using a small molecular polyol solution containing isopropyl acetate; combining the extracting solutions, and adding compound enzymes (cellulase, pectinase and subtilisin) for enzymolysis to obtain a crude extract; and finally, carrying out subcritical extraction and purification on the crude extract to obtain the product. Through improvement of extraction and purification processes, the extraction rate of active ingredients is effectively increased, a certain amount of glutathione is obtained, and toxicity is reduced; the invention also discovers that the composition ratio of the active ingredients of the extract obtained by the optimized process is in a proper range, and the anti-inflammatory and analgesic effects of the Kava pepper root extract are further improved.

The application discloses a method for preparing high-purity acrylic acid from a crude acrylic acid aqueous solution, and belongs to the technical field of acrylic acid purification. The method extracts the crude acrylic acid aqueous solution by using an extractant composed of isopropyl acetate and benzene or a derivative of benzene (toluene or xylene), so that the extractant is rich in acrylic acid, the types and contents of impurities in the extractant are reduced, and the recovery rate and purity of the acrylic acid are significantly improved.

The application discloses a method for synthesizing a tirofiban intermediate, and belongs to the technical field of drug synthesis. The method comprises the following steps: reacting chloroacetyl chloride and 1,2-difluorobenzene in dichloromethane as a solvent under the catalysis of aluminum chloride to obtain a TCAB-1 / 2 solution; performing enzyme catalytic reduction on the TCAB-1 / 2 solution to obtain a TCAB-3 mixed solution; dissolving the TCAB-3 mixed solution in toluene after concentration; condensing the TCAB-3 mixed solution in toluene in the presence of sodium tert-butoxide and triethyl phosphonoacetate to obtain a TCAB-4 toluene solution; performing ammination cyclization on the TCAB-4 toluene solution to obtain a TCAB-5 intermediate; mixing the TCAB-5 intermediate with liquid alkali, oxidizing the mixture by sodium hypochlorite, acidifying the mixture, extracting the mixture with isopropyl acetate to obtain an isopropyl acetate solution containing a TCAB-7 intermediate, and performing salt formation and crystallization on the isopropyl acetate solution to obtain the TCAB-7 intermediate. The method realizes the industrialized production of the tirofiban intermediate, is green and environment-friendly, has a simple route and controllable quality.

The application provides a refining method of a sacubitril valsartan sodium intermediate, and relates to the field of drug intermediate synthesis. The sacubitril valsartan sodium intermediate compound is (2R, 4S)-4-amino-5-(diphenyl-4-yl)-2-methylvalerate ethyl ester hydrochloride. The application also relates to a control method of specific impurities in the refining process of the compound, which comprises the following steps: mixing the sacubitril valsartan sodium intermediate crude product with ethyl acetate or isopropyl acetate, then heating to a reflux state, keeping the reflux state for 1-2 hours, and then performing slow cooling, pressure filtration, vacuum drying and other process procedures to obtain the sacubitril valsartan sodium intermediate (2R, 4S)-4-amino-5-(diphenyl-4-yl)-2-methylvalerate ethyl ester hydrochloride. The sacubitril valsartan sodium intermediate obtained by the refining method has high purity, no solvent residue, mild reaction conditions and is easy to be industrialized.

The present invention relates to solid forms I of N-(methoxycarbonyl)-3-methyl-L-valinyl-(4R)-N-{(1S)-1-cyano-2-[(3S)-2-oxopyrrolidin-3-yl] ethyl}-4-(trifluoromethyl)-L-prolinamide, in particular to solid forms I of N-(methoxycarbonyl)-3-methyl-L-valinyl-(4R)-N-{(1S)-1-cyano-2-[(3S)-2-oxopyrrolidin-3-yl The present invention relates to solid forms, such as anhydrous forms thereof, amorphous forms thereof, cyclopentyl methyl ether solvates thereof, isopropyl acetate solvates thereof, and ethyl acetate solvates thereof I and to pharmaceutical compositions comprising the solid forms and methods of treatment using the solid forms.

The invention provides a preparation method of waterborne polyurethane finish paint and the waterborne polyurethane finish paint, the waterborne polyurethane finish paint is prepared by self-modifying waterborne hydroxyl acrylic emulsion, waterborne polyurethane acrylate dispersion and L-tert-butyl aspartate under the combined action of isopropyl acetate, waterborne isocyanate, a coalescing agent, a wetting agent, deionized water and the like, and the waterborne polyurethane finish paint is prepared by self-modifying the waterborne hydroxyl acrylic emulsion, the waterborne polyurethane acrylate dispersion and the L-tert-butyl aspartate. The waterborne polyurethane finish paint which can be thickly coated and is good in anti-sagging performance, high in fullness and good in paint film glossiness is prepared.

The invention discloses a flame retardant and a preparation method thereof, and relates to the technical field of flame retardants, the flame retardant comprises a mixed flame retardant material composed of metal hydroxide, zinc borate, encapsulated red phosphorus and melamine cyanurate according to a mass ratio of 20-50: 5-15: 10-20: 5-10, and a silane coupling agent accounting for 0.8-1.2% of the total mass percentage; wherein the zinc borate is chitosan composite zinc borate, and the preparation method of the chitosan composite zinc borate comprises the following steps: mixing zinc borate, chitosan, zinc nitrate, water and isopropyl acetate, heating to 40-58 DEG C, reacting, then filtering and collecting to obtain the chitosan composite zinc borate after the temperature is reduced to room temperature. The flame retardant has the advantages of high flame-retardant efficiency, low cost, low smoke and low toxicity, and the binding capacity of the flame retardant and a rubber and plastic material and the flame-retardant property of the material are improved.

The invention discloses waste isopropyl acetate solution purification and recovery equipment and an operation method thereof, and belongs to the technical field of chemical waste liquid treatment.The waste isopropyl acetate solution purification and recovery equipment comprises a base and a filtering mechanism arranged on the base and used for filtering a waste isopropyl acetate solution, and the filtering mechanism comprises a filtering box, a liquid inlet pipe and a filtering part; the filter box is fixedly arranged on the top of the outer wall of the base, and the liquid inlet pipe is fixedly embedded in the top of the outer wall of the filter box. According to the waste isopropyl acetate solution purification and recovery equipment and the operation method thereof, large-particle impurities are preliminarily filtered through the first filter assembly, small-particle impurities are further filtered through the second filter assembly, double filtration is achieved, the purity of the solution is improved, interference of the impurities on the subsequent pH value adjustment and purification and recovery processes is reduced, and meanwhile, the purification and recovery efficiency of the waste isopropyl acetate solution is improved. The driving assembly enables the filtering part to rotate intermittently, multiple filtering plates, filtering nets and filtering cloth can be circularly switched, impurities are dispersed to the surfaces of the different filtering plates, the service life of the single filtering plate is prolonged, and the filtering efficiency is improved.

The invention discloses a chlorination reaction process in a sucralose preparation method, which comprises the following steps: reacting N-formyl-2-cyanopyrrolidine and oxalyl chloride in an acetylated tributyl citrate solvent under the reaction condition of 0-10 DEG C, and filtering, washing and drying after the reaction is finished to prepare N-chloromethylene-2-cyanopyrrolidine hydrochloride which is used as a chlorinating agent; respectively pumping an acetylated tributyl citrate solution of sucrose-6-ethyl ester and an acetylated tributyl citrate solution of the chlorinating agent into a continuous flow chlorination reaction system to obtain a chlorinated reaction solution; carrying out on-line membrane separation extraction on the chlorinated reaction liquid, and carrying out counter-current extraction by using isopropyl acetate to obtain an extraction phase and a reaction phase; and adsorbing, distilling and purifying the reaction phase, and recycling the recovered acetylated tributyl citrate solvent. According to the technical scheme, waste solvent discharge and waste water generation are reduced from the source, the three-waste treatment cost is reduced, and the economical efficiency and the environmental protection property of the whole process are improved.

The present invention discloses a sucralose-6-ester purification method, and particularly relates to the technical field of sucralose-6-ester purification, the method comprises: S1, crude product dissolution and adsorption refining: dissolving a crude product in a ternary complex solvent composed of isopropyl acetate, acetone and a poor solvent, and carrying out adsorption treatment by using mesoporous silica to obtain a refined filtrate, s2, programmed cooling crystallization: carrying out multi-stage programmed cooling crystallization including slow cooling crystal growing and rapid cooling crystallization on the refined filtrate, and inducing crystal precipitation, and S3, separating and drying: separating, washing and drying the obtained crystal to obtain a high-purity sucralose-6-ester product. According to the method, key impurities such as sucralose-4, 6-diester and the like are effectively removed through the synergistic effect of compound solvent refining, selective adsorption and programmed crystallization, the problem that the purity and the yield are difficult to consider at the same time is solved, the final product is high in purity and regular in crystal form, and a reliable guarantee is provided for preparation of high-quality sucralose.

The invention provides a method for synthesizing p-hydroxyacetophenone. The method comprises the following steps: producing phenyl acetate by using isopropyl acetate and phenol as raw materials; phenyl acetate is dissolved by using a mixed solvent, and a composite catalyst is adopted for catalysis, so that generation of by-products is reduced; gradient hydrolysis and purification are adopted, the yield and purity of the p-hydroxyacetophenone are effectively improved, and the p-hydroxyacetophenone prepared through the synthesis method has the advantages of being high in purity and yield; and the preparation method is simple and easy to control, simple in post-treatment process and suitable for industrial large-scale production.

The present disclosure relates to a process for the preparation of N-(methoxycarbonyl)-3-methyl-L-valinyl-(4R)-N-{(1S)-1-cyano-2-[(3S)-2-oxopyrrolidin-3-yl] ethyl}-4-(trifluoromethyl)-L-prolinamide, i.e., I, and forms thereof, and to a process for the preparation of N-(methoxycarbonyl)-3-methyl-L-valinyl-(4R)-N-{(1S)-1-cyano-2-[(3S)-2-oxopyrrolidin-3-yl] ethyl}- The present invention relates to compounds I, such as their Form 1 polymorphs, their cyclopentylmethyl ether solvates, their isopropyl acetate solvates, their ethyl acetate solvates, and mixtures of their Form 1 polymorphs with microcrystalline cellulose (I), and to compositions comprising solid forms, and to intermediates useful in the preparation of Compound I.

The invention relates to the technical field of medical materials, in particular to a borate disubstituted tyrosine derivative and a synthesis method and application thereof. The structural formula of the borate disubstituted tyrosine derivative is as shown in formula (I). The invention also provides a synthesis method of the borate disubstituted tyrosine derivative, which comprises the following steps: adding tyrosine into a solvent, cooling, adding di-tert-butyl dicarbonate, reacting to obtain a compound, dissolving the compound in dimethylformamide, adding N-halogenated succinimide, reacting to obtain a halogenated compound, dissolving the halogenated compound in the solvent, adding dimethyl sulfate and anhydrous potassium carbonate, reacting, filtering, washing and drying to obtain the borate disubstituted tyrosine derivative. And dissolving the intermediate halogenated compound in isopropyl acetate, adding potassium acetate, bis (pinacolato) diboron and a catalyst, reacting to obtain a compound, dissolving the compound in acid, and reacting to obtain the borate disubstituted tyrosine derivative. The invention also provides application of the borate disubstituted tyrosine derivative. The invention provides a novel boric acid-based tyrosine derivative, and solves the problem of low boron loading amount of the existing boron medicine. (I).

The invention relates to an analysis method for detecting multiple residual solvents in a medicine preparation process, which comprises the following steps of: simultaneously detecting methanol, tetrahydrofuran, ethanol, cyclohexane, diethyl ether, isopropyl acetate, acetone, n-heptane, isopropanol, n-butyl alcohol, acetonitrile, dioxane, dichloromethane, pyridine, tert-butyl alcohol, methylbenzene, tert-butyl methyl ether, N, N-dimethylformamide, N, N-dimethylformamide, N, N-dimethylformamide, N, N-dimethylformamide, N, N-dimethylformamide, N, N-dimethylformamide, N, N-dimethylformamide, N, N-dimethylformamide and N, N-dimethylformamide by adopting a gas chromatographic method; and 21 organic solvents including N, N-dimethylformamide, normal hexane, dimethyl sulfoxide and ethyl acetate are adopted. The method is not influenced by drug types, can be applied to content detection of various drug residual solvents, is simple to operate and wide in application, and saves drug detection time and detection cost.