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Production method of prednisone hydrolysate

A production process and hydrolyzate technology, applied in the direction of steroids, organic chemistry, etc., can solve the problems of low quality and yield of reactants, large amount of solvent, etc.

Active Publication Date: 2006-08-30
TIANJIN TIANYAO PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage is that a single solvent requires a large amount of solvent, and the quality and yield of the reactant are not high.

Method used

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  • Production method of prednisone hydrolysate

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Experimental program
Comparison scheme
Effect test

Embodiment approach 1

[0012] Throw in 60g of raw materials, 600-650ml of chloroform methanol (specific gravity 1.10-1.15), dissolve and clear, add 4-6% potassium hydroxide / methanol as a catalyst, react at 0-5°C for 30 minutes, neutralize and concentrate after the reaction is complete Crystallized, cooled, filtered, and dried to obtain 50 g of prednisone hydrolyzate, the liquid phase detection content was 97.8%, and the yield was 83.3%.

Embodiment approach 2

[0014] Throw in 60g of raw materials, 600-650ml of chloroform methanol (specific gravity 1.10-1.15), dissolve and clear, add 4-6% potassium hydroxide / methanol as a catalyst, react at 0-5°C for 30 minutes, neutralize and concentrate after the reaction is complete Crystallized, cooled, filtered, and dried to obtain 50.2 g of prednisone hydrolyzate, the liquid phase detection content was 98.2%, and the yield was 83.7%.

Embodiment approach 3

[0016] Throw in 60g of raw materials, 600-650ml of chloroform methanol (specific gravity 1.10-1.15), dissolve and clear, add 4-6% potassium hydroxide / methanol as a catalyst, react at 0-5°C for 30 minutes, neutralize and concentrate after the reaction is complete Crystallized, cooled, filtered, and dried to obtain 50.5 g of prednisone hydrolyzate, the liquid phase detection content was 98.2%, and the yield was 84.2%.

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Abstract

The present invention relates to a production method of prednisone hydrolysate. Said production method includes the following steps: using intermediate prednisone acetate as raw material, using chloroform and methyl alcohol mixed solution as solvent, using potassium hydroxide solution as catalyst, making them be reacted at low temperature, neutralizing, concentrating to make crystallization, cooling, filtering and drying so as to obtain the prednisone hydrolysate. Said invention can raise its yield and quality.

Description

Technical field: [0001] The invention relates to a production process of prednisone hydrolyzate. Background technique: [0002] The traditional production process of prednisone hydrolyzate uses a single solvent methanol as a solvent, solid potassium hydroxide as a catalyst, and reacts at 24--26 ° C. After the reaction is completed, it is neutralized, concentrated and crystallized, cooled, filtered, and dried to obtain Prednisone hydrolyzate. The disadvantage is that a single solvent requires a large amount of solvent, and the quality and yield of reactants are not high. Invention content: [0003] The present invention is aimed at the problem that prior art exists, provides a kind of production technology method of prednisone hydrolyzate, with chloroform: methanol is solvent, potassium hydroxide / methanol is catalyst, low temperature is reacted, and product quality and yield have been obtained improve. [0004] In order to realize the purpose of the present invention, pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J7/00
Inventor 王琼尧赵一兵
Owner TIANJIN TIANYAO PHARM CO LTD
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