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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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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 jacket heating distillation, the heat conduction surface is small, the distilling efficiency is low, and the product quality yield is mostly in the 74-78%, the product yield has never exceeded 81%, and the content of main impurities in the product is high

Method used

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Experimental program
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Embodiment Construction

[0019] 1. Oximation reaction.

[0020] (1) Specifications and proportions of raw materials used.

[0021] Dienolone acetate: toluene+ethanol:pyridine:hydroxylamine hydrochloride=1:3:0.4:0.213, wherein 160kg dienolone acetate, 320kg+160kg toluene+ethanol, 64kg pyridine, and 34kg hydroxylamine hydrochloride.

[0022] (2) Process operation.

[0023] First put hydroxylamine hydrochloride and pyridine into 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 acetic acid gestational dienolone, heat and reflux for 3 hours, cool and crystallize, and put it in a centrifuge Carry out centrifugal drying in the machine sink, recover the mother liquor and use it next time, rinse the reaction solution with warm water until there is no foam, centrifugal drying, and dry until the water content is below 0.2%, that is, the acetic acid pregnant dienol ketone oxime (oximide) 163kg, the content is 99%,...

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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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