Preparation method for 9,11-de-esterification of metllylpredllisolone series products

A technology for methylprednisolone and series products, which is applied in the field of methylprednisolone series products 9,11—deesterification production technology, and can solve the problem of destroying the structure of the target product, fluctuation of the reaction reflux temperature, and low quality and yield of the main product. and other problems to achieve the effect of reducing the degree of damage, stable reflux temperature, and improving quality and yield

Active Publication Date: 2007-02-07
TIANJIN TIANYAO PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Its disadvantages are: this process adopts sulfonylate wet product feeding, the water content of sulfonylate is unstable, and the ratio of acetic acid to water after dissolution is indeterminate, which makes the reaction reflux temperature fluctuate up and down. If the temperature is too high, the structure of the target product will be destroyed, resulting in Main product quality and yield are low

Method used

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  • Preparation method for 9,11-de-esterification of metllylpredllisolone series products
  • Preparation method for 9,11-de-esterification of metllylpredllisolone series products

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Embodiment 1

[0020] Embodiment 1: react with dehydrogenate 10g and a certain amount of methanesulfonyl chloride, after completion of the reaction, get sulfonylate wet product 16.7g, react with 60g acetic acid, 25-30g sodium acetate and sulfonylate, heat up to Fully reflux, the reflux temperature is 115°C, after the reaction is completed, dilute, filter, and dry to obtain 8.4 g of methylprednisolone 9,11-desesterified product, the content is 82.2%, and the yield is 84.0%.

Embodiment 2

[0021] Embodiment 2: react with dehydrogenate 10g and a certain amount of methanesulfonyl chloride, after completion of the reaction, get sulfonylate wet product 16.5g, react with 60g acetic acid, 25-30g sodium acetate and sulfonylate, heat up to Fully reflux, add 6.5ml of temperature-controlled water, the reflux temperature is 109°C, after the reaction is completed, dilute, filter, and dry to obtain 8.84g of methylprednisolone 9,11-desesterified product, the content is 86.2%, and the yield is 88.0%.

Embodiment 3

[0022] Embodiment 3: react with dehydrogenate 10g and a certain amount of methanesulfonyl chloride, after completion of the reaction, get sulfonylate wet product 16.9g, react with 60g acetic acid, 25-30g sodium acetate and sulfonylate, heat up to Fully reflux, add 7.5ml of temperature-controlled water, the reflux temperature is 107.5°C, after the reaction is completed, dilute, filter, and dry to obtain 8.75g of methylprednisolone 9,11-desesterified product, the content is 86.7%, and the yield is 87.0%.

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Abstract

The invention discloses a manufacturing method of 9, 11-deestering material, which comprises the following steps: adopting intermediate dehydrogenation as raw material; proceeding sulfur-esterifying reaction through dansyl chloride; diluting; filtering; obtaining the wet product; heating to reflux completely; complementing temperature-control water; adjusting reflux reaction at 109+-2 deg.c; diluting; filtering; drying to obtain methylprednisolone 9, 11- deestering material.

Description

Technical field: [0001] The invention relates to a production process of methylprednisolone series products 9, 11 --- deesterified products. Background technique: [0002] The traditional production process of methylprednisolone 9,11-deesterification product uses intermediate 11-sulfonate wet product, acetic acid and potassium acetate as raw materials to carry out 9,11-deesterification reaction, rapidly heats up to full reflux, and reacts After completion, dilute, filter, and dry to obtain methylprednisolone 9,11-desesterified product. Its disadvantages are: this process adopts sulfonylate wet product feeding, the water content of sulfonylate is unstable, and the ratio of acetic acid to water after dissolution is indeterminate, which makes the reaction reflux temperature fluctuate up and down. If the temperature is too high, the structure of the target product will be destroyed, resulting in The main product quality and yield are low. Invention content: [0003] The pres...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J7/00
Inventor 卢彦昌李金禄孙亮
Owner TIANJIN TIANYAO PHARM CO LTD
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