Dehydroepiandrosterone acetate preparation method

A technology for dehydroepiandrosterone acetate and gestational dienolone acetate is applied in the field of preparation of dehydroepiandrosterone acetate, which can solve the problems of chloroform toxicity, carcinogenicity, high content of main impurities, low distillation efficiency and the like, and achieves the The effect of shortening the reaction time, speeding up the reaction process, and improving the solubility

Inactive Publication Date: 2014-10-15
JIANGXI CHENYANG PHARMA CO LTD
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  • Summary
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AI Technical Summary

Problems solved by technology

However, chloroform is toxic and carcinogenic
[0004] Moreover, in the traditional preparation method, the washing and distilling link of producing dehydroepiandrosterone acetate from the raw material acetic acid dienolone adopts the reaction kettle jack

Method used

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Examples

Experimental program
Comparison scheme
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Example Embodiment

[0019] 1. The oximation reaction.

[0020] (1) Specification and ratio of raw materials used.

[0021] Pregnancy dienolone acetate: toluene + ethanol: pyridine: hydroxylamine hydrochloride = 1:3:0.4:0.213, of which pregnancy dienolone acetate 160 kg, toluene + ethanol 320 kg + 160 kg, pyridine 64 kg, hydroxylamine hydrochloride 34 kg.

[0022] (2) Process operation.

[0023] Put hydroxylamine hydrochloride and pyridine in a 1000L oximation tank, then pump in a mixed solvent of toluene and ethanol, stir and heat until the reaction solution is completely dissolved, add gestation dienolone acetate, heat to reflux for 3 hours, cool to crystallize, and centrifuge Centrifugal drying is carried out in the machine sink, the mother liquor is recovered for the next application, the reaction liquid is washed with warm water until there is no foam, centrifuged and dried, and dried until the moisture content is below 0.2%, and the pregnancy dienol ketoxime acetate (oxime) is obtained. 163kg, the ...

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Abstract

A dehydroepiandrosterone acetate preparation method relates to the technical field of preparation of a steroid hormone drug medical intermediate. Dehydropregnenolone acetate is used as a raw material, a toluene and ethanol mixed solvent is used as a reaction solvent, then dehydropregnenolone acetate oxime is obtained by oximation reaction, cooling crystallization, centrifugation, water washing and drying; a dehydroepiandrosterone acetate crude product is obtained by rearrangement hydrolysis reaction, water washing rushed distillation, centrifugation and drying; and a dehydroepiandrosterone acetate fine product is obtained by decolouring refining, filtration, concentration and crystallization and drying of the crude product. According to the method, the solubility of the dehydropregnenolone acetate and oxime is greatly improved, the reaction is more complete, and methyl in the toluene can be transformed into carboxyl group in the human body, so that the toluene can be transformed into benzoic acid to be excreted the body, and the dehydroepiandrosterone acetate is non-toxic.

Description

technical field [0001] The invention relates to the technical field of preparation of steroid hormone pharmaceutical intermediates, in particular to a preparation method of dehydroepiandrosterone acetate. Background technique [0002] Dehydroepiandrosterone acetate, chemical name 3-β-hydroxy-deoxyandrost-5-ene-17-one-3-acetate, Chinese alias is also called rearrangement, dehydroepiandrosterone acetate, is It is an important intermediate for the synthesis of various hormones, family planning products and other steroid hormone drugs. At present, the traditional preparation method of dehydroepiandrosterone acetate is as follows: take dienolone acetate as raw material, use ethanol as solvent, carry out oximation reaction with hydroxylamine hydrochloride, cool and crystallize, centrifugally dry, wash with water, and dry to obtain Acetic acid pregnant dienol ketone oxime; then use pure benzene as a solvent, carry out rearrangement reaction with phosphorus oxychloride, then carry ...

Claims

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Application Information

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IPC IPC(8): C07J1/00
Inventor 王日进成润泽
Owner JIANGXI CHENYANG PHARMA CO LTD
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