Technology for refining 4-androstenedione from dehydroepiandrosterone mother solution

A technology of dehydroepiandrosterone and androstenedione, which is applied in the field of processing dehydroepiandrosterone mother liquor, can solve the problems of low yield of 4-androstenedione, and achieve environmental protection and reduce solid The effect of waste discharge

Inactive Publication Date: 2016-07-27
湖北省丹江口开泰激素有限责任公司
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  • Description
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AI Technical Summary

Problems solved by technology

The method for extracting 4-androstenedione from the DHEA mother liquor in the prior art is to first separate the DHEA mother liquor by column chromatography, and then synthesize the separated material into 4-androstenedione, and the 4-androstenedione obtained by the above refining method Diketone yield is low

Method used

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  • Technology for refining 4-androstenedione from dehydroepiandrosterone mother solution

Examples

Experimental program
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Effect test

Embodiment 1

[0037] S1, take 100kg of dehydroepiandrosterone mother liquor obtained in the process of synthesizing dehydroepiandrosterone with 4-androstenedione, add 1000kg of toluene, heat and dissolve it at 50°C, and use 20kg of methanol + 180kg of water + 20kg of hydrochloric acid to form Adjust the pH value of the solution to 2, stir at 55°C for half an hour, separate the water in the lower layer, and wash the upper layer with hot water until the pH is 7;

[0038] S2, heating the upper layer liquid obtained in step S1 to 112°C, reflux for dehydration, then lower the temperature to 80°C, add cyclohexanone, and reflux for dehydration until the effluent is clear;

[0039] S3, after the dehydration is completed, cool down to 110°C, add aluminum isopropoxide, slowly raise the temperature to 114°C, react for 5 hours, take samples for TLC spot detection until the reaction is complete;

[0040] S4, after the reaction is completed, lower the temperature to 80°C, add NaOH aqueous solution, and r...

Embodiment 2

[0045] S1, take 100kg of dehydroepiandrosterone mother liquor obtained in the process of synthesizing dehydroepiandrosterone with 4-androstenedione, add 1000kg of ethyl acetate, heat and dissolve at 50°C, use 30kg of ethanol + 280kg of water + 30kg The acid solution composed of hydrochloric acid adjusts the pH value of the solution to 2.5, stirs at 52°C for half an hour, separates the water in the lower layer, and washes the upper layer with hot water until the pH is 6.5;

[0046] S2, heating the upper layer liquid obtained in step S1 to 111°C, reflux for dehydration, then lower the temperature to 85°C, add cyclohexanone, and reflux for dehydration until the effluent is clear;

[0047] S3, after the dehydration is completed, cool down to 105°C, add aluminum isopropoxide, slowly raise the temperature to 112°C, react for 6 hours, take samples for TLC spot detection until the reaction is complete;

[0048] S4, after the reaction is completed, lower the temperature to 85°C, add Na...

Embodiment 3

[0053] S1, take 100kg of dehydroepiandrosterone mother liquor obtained in the process of synthesizing dehydroepiandrosterone with 4-androstenedione, add 1000kg of ethyl acetate, heat and dissolve at 55°C, use 50kg of ethanol + 480kg of water + 50kg The acid solution composed of hydrochloric acid adjusts the pH value of the solution to 3, stirs at 55°C for half an hour, separates the water in the lower layer, and washes the upper layer with hot water until the pH is 7;

[0054] S2, heating the supernatant liquid obtained in step S1 to 112°C, reflux for dehydration, then lower the temperature to 90°C, add calcium hypochlorite, and reflux for dehydration until the effluent is clear;

[0055] S3, after the dehydration is completed, cool down to 110°C, add aluminum isopropoxide, slowly raise the temperature to 114°C, react for 8 hours, take samples for TLC spot detection until the reaction is complete;

[0056] S4, after the reaction is completed, lower the temperature to 90°C, add...

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Abstract

The invention discloses a technology for refining 4-androstenedione from a dehydroepiandrosterone mother solution. The technology comprises the steps that dehydroepiandrosterone is pretreated, reflux dehydration, addition of a weak oxidant, reflux dehydration and addition of aluminum isopropoxide for a reaction are carried out in sequence, an alkaline aqueous solution is added for a reaction, washing and distillation are carried out, and crude 4-androstenedione is obtained; then refining and purifying are carried out, and the 4-androstenedione product high in purity and yield is obtained.

Description

technical field [0001] The invention relates to a treatment method for dehydroepiandrosterone mother liquor, in particular to a process for refining 4-androstenedione from dehydroepiandrosterone mother liquor. Background technique [0002] Dehydroepiandrosterone, chemical name: 3β-hydroxy-5-androsten-17-one, namely DHEA, 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...

Claims

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Application Information

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IPC IPC(8): C07J1/00
CPCC07J1/0011
Inventor 闻开学陈春笋
Owner 湖北省丹江口开泰激素有限责任公司
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