Method for recovering 16-dehydropregnenolone acetate from 16-dehydropregnenolone acetate mother liquor

A technology of dienolone acetate and mother liquor, which is applied in the direction of steroids and organic chemistry, can solve the problems of complex chemical reactions, affecting product quality and yield, and difficult control, and achieves simple process operation, easy industrialization, The effect of high utilization

Inactive Publication Date: 2014-02-05
XIANGXI HUALI PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main reasons are as follows: First, due to the existence of a large number of diene alcohol isomers, high polymers, inorganic substances and organic acids in the mother liquor, the chemical reaction of the entire diene process is more complicated and difficult to control during the mechanical application process. Affect product quality and yield; Second, because the diene mother liquor is applied in the ring-opening reaction process, affected by high temperature and high pressure conditions, the diene in the mother liquor is

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] 100kg of diosgenin was fed into the dienolone acetate mother liquor obtained after catalytic ring-opening, oxidation and hydrolysis synthesis to obtain 80kg of concentrated mother liquor (dienolone acetate content 13.4%, HPLC external standard method) after concentration. Stir 300kg of cyclohexane at 60°C for 60min, let it stand for 15min, cool the supernatant to 30°C, then use 100kg of cyclohexane to operate twice in the same way, and combine the supernatant. Pack the column with 100kg of silica gel, pass the supernatant through the column, and collect the chromatographic solution. Concentrate the chromatographic liquid at 75°C until there is no liquid, and remove the residual solvent with 12 kg of 95% ethanol. Reflux with 100kg of 95% ethanol at 85°C for 90 minutes, cool naturally to room temperature, then freeze to 5°C and keep for 48 hours, naturally warm to 9°C, centrifuge, wash with 9°C mass fraction of 95% ethanol until milky white, and dry at 85°C , weighing 8....

Embodiment 2

[0030] Dienolone acetate mother liquor obtained after 100kg of diosgenin was fed through catalytic ring-opening, oxidation and hydrolysis synthesis was concentrated to obtain 78.5kg of concentrated mother liquor (dienolone acetate content 14.1%, HPLC external standard method), Stir with 310kg cyclohexane at 62°C for 60min, let it stand for 18min, cool the supernatant to 28°C, then use 100kg cyclohexane to operate twice in the same way, and combine the supernatant. Pack the column with 90kg of silica gel, pass the supernatant through the column, and collect the chromatographic solution. The chromatographic solution was concentrated at 78°C until there was no liquid, and the residual solvent was removed with 14 kg of 95% ethanol. Reflux with 95kg of 95% ethanol at 80°C for 120 minutes, cool to room temperature naturally, then freeze to 6°C and keep for 48 hours, naturally warm to 8°C, centrifuge, wash with 95% ethanol at 6°C until milky white, and dry at 85°C , weighing 8.27kg ...

Embodiment 3

[0032] 100kg of diosgenin was fed into catalyzed ring-opening, oxidized, and hydrolyzed to produce the dienolone acetate mother liquor obtained after concentration to obtain 80kg of concentrated mother liquor (dienolone acetate content 12.9%, HPLC external standard method). Stir 300kg of petroleum ether at 58°C for 60min, let it stand for 22min, cool the supernatant to 25°C, then use 100kg of petroleum ether in the same way twice, and combine the supernatant. Pack the column with 100kg of silica gel, pass the supernatant through the column, and collect the chromatographic solution. Concentrate the chromatographic liquid at 70°C until there is no liquid, and remove the residual solvent with 15 kg of 95% ethanol. Reflux with 105kg of 95% ethanol at 86°C for 90 minutes, cool naturally to room temperature, then freeze to 5°C and keep for 72 hours, naturally warm to 10°C, centrifuge, wash with 5°C mass fraction of 95% ethanol until milky white, and dry at 80°C , weighing 7.74kg pu...

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Abstract

The invention relates to a method for recovering 16-dehydropregnenolone acetate from a 16-dehydropregnenolone acetate mother liquor, wherein the method is intended to provide the method with advantages of simple technology, high recovery rate and good product quality. The method for recovering 16-dehydropregnenolone acetate from the 16-dehydropregnenolone acetate mother liquor comprises the following steps of: mother liquor condensation, solvent extraction, chromatography to remove impurities, condensation of a chromatography liquid, refining, crystallization, centrifugation and drying, to obtain 16-dehydropregnenolone acetate. The method for recovering 16-dehydropregnenolone acetate from the 16-dehydropregnenolone acetate mother liquor can make an overall yield of the 16-dehydropregnenolone acetate reach 72%, raising 4-7% compared with a traditional technology; a used reagent belongs to a common chemical product, and has advantages of easy availability, low cost, simple technology operation and convenient industrialization; and the method is used for recovering the 16-dehydropregnenolone acetate from the 16-dehydropregnenolone acetate mother liquor, wherein the purity of the 16-dehydropregnenolone acetate obtained after refining is larger than 99%, the obtained 16-dehydropregnenolone acetate can be directly used as a product, and a secondary mother liquor can be reused into the 16-dehydropregnenolone acetate production.

Description

technical field [0001] The invention relates to a method for recovering dienes, in particular to a method for recovering dienes from dienolone acetate mother liquor. Background technique [0002] Dienolone acetate (referred to as diene), chemical name: 3β-hydroxy-pregna-5,16-diene-20-one-3-acetate, it is an important intermediate for the synthesis of steroid hormone APIs It can be used as a raw material to produce adrenal hormone drugs, glucocorticoid drugs, steroidal anti-inflammatory drugs, sex hormone drugs, and oral contraceptives for women. Dienolone acetate mother liquor (referred to as diene mother liquor) is a liquid obtained by catalyzing ring-opening, oxidation, and hydrolysis of diosgenin to synthesize dienolone acetate, and then centrifuging and washing. After recovering the residual solvent, the mother liquor still contains a large amount of dienes, so it is usually treated before being used. [0003] At present, in the prior art, the diene mother liquor is us...

Claims

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Application Information

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IPC IPC(8): C07J13/00
Inventor 彭光花吴正良饶洁樊学明全铁传刘永源王余兵
Owner XIANGXI HUALI PHARMA
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