A kind of method for recovering diene from dienolone acetate mother liquor

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...

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 damaged twice, thereby affecting the yield; Third, conventional mother liquor treatment adopts The method of saponification treatment, in which part of the dienolone acetate will react to form a dienol compound, and only 30-40% of the compound is converted into a dienolone acetate in the ring-opening process, and the remaining alcohol form The compound exists as a by-product in the whole process; the fourth is that some other by-products that can undergo reversible reactions cannot be 100% converted into dienes in the reaction.