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Method for processing dehydroepiandrosterone mother liquor objects

A technology of dehydroepiandrosterone and a treatment method, applied in the directions of steroids, organic chemistry, etc., can solve problems such as pollution of the environment, and achieve the effects of high utilization rate and pollution reduction.

Active Publication Date: 2015-06-10
湖北竹溪人福药业有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the prior art, the treatment method of DHEA mother liquor is to concentrate the solvent to a certain volume, lower the temperature to precipitate DHEA, and then filter it, and obtain a small amount of DHEA through refining for many times. During this process, part of DHEA and Steroidal materials such as 3α-hydroxy-5-androsten-17-one and 3,17-bisketal always exist in the mother liquor, and the materials are not fully utilized and pollute the environment

Method used

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  • Method for processing dehydroepiandrosterone mother liquor objects
  • Method for processing dehydroepiandrosterone mother liquor objects

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Experimental program
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Effect test

Embodiment 1

[0031] 100g of 4-AD sample was taken, refined through esterification, ketalization, reduction, and hydrolysis to obtain 66g of dehydroepiandrosterone (HPLC: 99.6%) and 30g of dehydroepiandrosterone mother liquor (dry weight). Stir and dissolve the mother liquor with 30ml of dichloromethane. The eluent is: petroleum ether: ethyl acetate = 3:1. The mother liquor is separated by column chromatography and collected in sections, monitored by TLC. Combine the same components, concentrate and dry the chromatographic solution, and dry the sample to obtain 10g dehydroepiandrosterone (HPLC: 99.6%), 8g 3α-hydroxyl-5-androsten-17-one, 5g3,17-bis Ketones.

[0032] Accurately measure 32ml of ethyl acetate, add 24ml of glacial acetic acid into the reaction flask, add 8g of 3α-hydroxy-5-androsten-17-one obtained by passing through the column, stir and dissolve, add 2g of calcium hypochlorite to the reaction flask, 30 Temperature control reaction at ℃ for 1h, TLC spotting until the raw materi...

Embodiment 2

[0035] Take 200g 4-AD sample, undergo esterification, ketalization, reduction, and hydrolysis to obtain 130g dehydroepiandrosterone (HPLC: 99.7%) and 60g mother liquor (dry weight). Stir and dissolve the mother liquor with 90ml of dichloromethane, the eluent is: petroleum ether: ethyl acetate = 4:1, collect the chromatographic solution through the column, concentrate and dry the chromatographic solution, and dry the sample at 50-60°C to obtain 20g of Hydroepiandrosterone (HPLC: 99.5%), 18 g of 3α-hydroxy-5-androsten-17-one, 10 g of 3,17-bisketal.

[0036] Accurately measure 90ml of ethyl acetate, add 72ml of glacial acetic acid into the reaction flask, add to the reaction flask, add 18g of 3α-hydroxy-5-androsten-17-one obtained through the column, stir to dissolve, and add 5.04g of Calcium hypochlorite, react at 20°C for 2 hours, spot on TLC plate until the reaction of the raw materials is complete, add 3.6g of sodium bisulfite and stir for 15min, add 270ml of water and stir f...

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Abstract

The invention discloses a method for processing dehydroepiandrosterone mother liquor objects. DHEA, 3alpha-hydroxide radical-5-androstene-17-ketone and 3, 17-diketal objects can be obtained through column chromatography isolation; then the obtained 3alpha-hydroxide radical-5-androstene-17-ketone and the obtained 3, 17-diketal objects synthesize a starting material 4-AD. By means of the method, the purity of the dehydroepiandrosterone (DHEA) obtained through the column chromatography isolation is larger than or equal to 99.5%, and the DHEA total yield is larger than or equal to 75%; materials obtained through the column chromatography isolation can synthesize the 4-AD, reusing can be carried out, and the using rate is high; pollution of hormone waste to the environment is reduced.

Description

technical field [0001] The invention relates to a method for treating dehydroepiandrosterone mother liquor. Background technique [0002] Dehydroepiandrosterone, English name: Dehydroepiandrosterone, chemical name: 3β-hydroxy-5-androsten-17-one, molecular formula C 19 h 28 o 2 . DHEA is an important intermediate and raw material for the manufacture of steroid hormone drugs, and it has anti-aging and protein assimilation effects. [0003] Domestic manufacturers of dehydroepiandrosterone used to use diosgenin or pendirolone to obtain dehydroepiandrosterone through ring-opening acylation, oxidative hydrolysis, oximation, Beckmann rearrangement hydrolysis, and hydrolysis. , the process route is long, the raw material saponin is highly regional, the resources are limited, the production cost is high, the operation is cumbersome, and the environment is polluted greatly. [0004] In recent years, more and more scholars use phytosterol fermentation product 4-AD as raw material ...

Claims

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Application Information

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IPC IPC(8): C07J1/00
CPCC07J1/0011
Inventor 周建生杨艳青郑建雄常文胜侯海波
Owner 湖北竹溪人福药业有限责任公司
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