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Method for aqueous phase oxo-synthesis of Iansoprazole

A technology of oxidative synthesis and lansoprazole, applied in the direction of organic chemistry, can solve the problems of expensive, difficult to recycle, flammable, etc., and achieve the effect of low cost, good yield, and high chemical purity

Active Publication Date: 2007-02-28
YOUCARE PHARMA GROUP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Lansoprazole has relatively mature synthetic method at present, and has been put into large-scale industrial production, but all is to adopt organic solvent in oxidative synthesis reaction, as: methylene chloride, ethyl acetate etc.; These solvents are all difficult to reclaim, and price expensive, toxic and flammable

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Weigh 6.2028 g of citric acid in a beaker, add 20 ml of distilled water to dissolve, stir with a glass rod for about five minutes, and then completely dissolve the citric acid to obtain a citric acid solution (a colorless and transparent solution). Get a 50ml round-bottomed flask, put a stirring bar, and 0.882g of 2-[3-methyl-4-(2,2,2-trifluoroethoxy)-2-pyridyl]sulfide-1H - Add benzimidazole into the flask with a glass funnel, add citric acid solution, stir to allow it to react. When the citric acid solution was just added, 2-[3-methyl-4-(2,2,2-trifluoroethoxy)-2-pyridyl]sulfide-1H-benzimidazole was insoluble and floated On the surface of the citric acid solution; after reacting for 3 hours, the solution was clear and transparent and completely dissolved. Place the flask in the refrigerator to freeze.

[0024] Take out the flask from the refrigerator, the liquid in the flask is completely frozen, let stand, and thaw at room temperature. After 30 minutes, the ice cube...

Embodiment 2

[0028] Pipette 20ml of glacial acetic acid into the flask, add 80ml of distilled water to dissolve, then add 6g of 2-[3-methyl-4-(2,2,2-trifluoroethoxy)-2-pyridyl]sulfide group- 1H-benzimidazole was added to the flask, stirred and dissolved to obtain a clear solution, and 10ml of hydrogen peroxide solution with a mass concentration of 30% was added dropwise in an ice-water bath. After reacting for 2 hours, ammonia water was added dropwise to adjust the pH value of the solution. White matter precipitated out, and when the pH of the system was 8, the dropwise addition of aqueous ammonia was stopped.

[0029] Use a Buchner funnel for suction filtration to obtain a white filter cake, wash the filter cake with water until neutral, put the filter cake into a small beaker, and freeze in the refrigerator. After one hour, the beaker was removed and dried in a vacuum freeze dryer. The temperature of the cold trap was -48°C. Take out the beaker after 5 hours, weigh medicine (being lans...

Embodiment 3

[0031] Add 80ml of water to the flask, pipette 10ml (ml) of 1mol / L sulfuric acid into the flask, then add 6g of 2-[3-methyl-4-(2,2,2-trifluoroethoxy)-2- Pyridyl] thioether-1H-benzimidazole in the flask, stirring and dissolving, after 5 minutes, a clear solution was obtained, and 5ml volume concentration was added dropwise in an ice-water bath as an aqueous solution of 10% peracetic acid, and after 2 hours of reaction, Add dropwise sodium hydroxide aqueous solution (mass concentration is 10%), adjust the pH value of the solution, the system has white matter to separate out gradually, when the pH of the system is about 8, stop dripping the sodium hydroxide aqueous solution.

[0032] Use a Buchner funnel for suction filtration to obtain a white filter cake, wash the filter cake with water until neutral, put the filter cake into a small beaker, and freeze in the refrigerator. After one hour, the beaker was removed and dried in a vacuum freeze dryer. The temperature of the cold tr...

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PUM

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Abstract

The invention discloses a preparing method of lansuola pyrazole, which comprises the following steps: 1) selecting solvent A and water compound solvent B; allocating 2-97% solvent B and 3-98% 2-[3-methyl-4-(2,2,2-trifluoro ethyoxyl)-2-pyridine] sulfide-H-benzimidazole to prepare compound C; 2) blending 0-30% solvent D, 0-80% water and 20-100% oxidant to prepare compound E with the molar rate of oxidant and 2-[3-methyl-4-(2,2,2-trifluoro ethyoxyl)-2-pyridine] sulfide-H-benzimidazole at 0.1-10:1; 3) blending compound C and compound E under -10-50 deg.c; 4) adjusting pH value of composite solution at 5-11 through acid or alkaline; separating to obtain the product.

Description

technical field [0001] The present invention relates to a kind of preparation method of lansoprazole, particularly relate to a kind of preparation method of aqueous phase oxidation synthesis lansoprazole. Background technique [0002] Lansoprazole (English name: Lansoprazole, trade name AG-1749), chemical name: (±)-2[[[3-methyl-4-(2,2,2-trifluoroethoxy)- 2-Pyridyl]methyl]sulfinyl]-1H-benzimidazole is a proton pump inhibitor developed by Takeda Corporation of Japan. At the end of 1991, Takeda Corporation and French Houde Company were jointly approved to be marketed in France. It is used for twelve Short-term treatment of duodenal ulcers and reflux esophagitis. The drug is the second proton pump inhibitor on the market after omeprazole (Omeprazole). Lansoprazole is the benzimidazole derivative of replacement, has introduced trifluoroethoxyl group on the 4-position of pyridine ring (it is reported that Lansoprazole is owing to introducing fluorine in its chemical structure, t...

Claims

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Application Information

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IPC IPC(8): C07D401/12C07D235/00C07D213/00
Inventor 陈金芳陈启明邵寿强
Owner YOUCARE PHARMA GROUP
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