Preparation method of dydrogesterone intermediate diene ketal

A technology of diene ketal and dydrogesterone is applied in the field of preparation of diene ketal, which can solve the problems of complex preparation method and low preparation efficiency, and achieve the effect of simple and efficient preparation method

Inactive Publication Date: 2019-09-06
ZHEJIANG SHENZHOU PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Aiming at the deficiencies of the prior art, the present invention provides a method for the preparation of dydrogesterone intermediate diene ketal, which has the advantages of being simple and efficient, suitable for large-scale industrial production, etc. The preparation method is complicated and the preparation efficiency is low

Method used

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  • Preparation method of dydrogesterone intermediate diene ketal
  • Preparation method of dydrogesterone intermediate diene ketal

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Effect test

Embodiment 1

[0022] A preparation method of a dydrogesterone intermediate diene ketal, comprising the following processing steps:

[0023] Add 10 grams of 7α-hydroxyprogesterone and 0.5 grams of p-toluenesulfonic acid to 20 milliliters of ethylene glycol, and react at a controlled temperature of 25°C for 6 hours, add an appropriate amount of triethylamine, cool down to 0°C, filter, and dry to obtain a ketal product 11.5 grams.

Embodiment 2

[0025] A preparation method of a dydrogesterone intermediate diene ketal, comprising the following processing steps:

[0026] Add 10 grams of 7α-hydroxyprogesterone and 0.5 grams of pyridinium hydrobromide to 20 milliliters of ethylene glycol, react at a controlled temperature of 30°C for 8 hours, add an appropriate amount of pyridine, lower the temperature to 0°C, filter, and dry to obtain ketal product 11.6 gram.

Embodiment 3

[0028] A preparation method of a dydrogesterone intermediate diene ketal, comprising the following processing steps:

[0029] Add 10 grams of 7α-hydroxyprogesterone, 10 milliliters of ethylene glycol and 0.5 grams of pyridine hydrochloride to 20 milliliters of dichloromethane, control the temperature at 25 ° C for 7 hours, add an appropriate amount of pyridine, concentrate the dichloromethane, cool to 0 ° C, Filter and dry to obtain 11.3 g of ketal product.

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Abstract

The invention relates to the technical field of preparation of diene ketal, and particularly discloses a preparation method of a dydrogesterone intermediate diene ketal. 7alpha-hydroxyprogesterone isinvolved; the preparation method comprises the steps that 1, the 7alpha-hydroxyprogesterone is taken and put into a glass beaker; 2, an organic solvent is added to the glass beaker, and the glass beaker is subjected to water bath heating; 3, an acid catalyst is added to the glass beaker in step 2, and water bath heating continues; 4, a placement reaction is carried out, the reaction time is 4-8 hours, and therefore ketal can be obtained; 5, a certain quantity of a reaction solvent is added in the ketal obtained in step 4, and concentration and purification are carried out to obtain the diene ketal. The preparation method of the dydrogesterone intermediate diene ketal has the advantages that the 7alpha-hydroxyprogesterone can be subjected to a ketal reaction and a dehydroxylation reaction to quickly prepare the diene ketal, and the preparation method is simple, efficient, suitable for industrialized production and convenient to use by people.

Description

technical field [0001] The invention relates to the technical field of preparation of diene ketals, in particular to a method for preparing a dienyl ketal intermediate of dydrogesterone. Background technique [0002] Dydrogesterone, whose chemical name is (9β,10α)-Pregna-4,6-diene-3,20-dione, is a progestin and can be used clinically to treat amenorrhea, endometriosis, and prevent functional bleeding and threatened abortion. Among the synthetic progestogens currently used clinically, dehydroprogesterone is superior to other similar drugs, and it is an effective and orally active synthetic progesterone drug. [0003] With the increasing use of dydrogesterone, the amount of dydrogesterone used is increasing. At present, dydrogesterone is generally prepared from dien ketals through photoreaction and hydrolysis. Diene ketals in the prior art generally need to be prepared through multiple reactions such as cyanide reaction, ketal reaction, etherification Grignard reaction, oxida...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J71/00
CPCC07J71/0026
Inventor 王友富王荣王炳乾王洪福邵振平雷灵芝黄橙橙王瑞陈克纲应杨波
Owner ZHEJIANG SHENZHOU PHARMA
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