Method for producing high purity diene alcohol ketone acetic ester

Abstract

The invention provides a method for producing dehydropregnenolone acetate with high purity. The method takes diosgenin as a raw material, and comprises the steps of pressure pyrolysis, oxidation, hydrolysis, extraction, column fractionation, and condensation. Compared with the traditional method for producing the dehydropregnenolone acetate, particularly the treating process of mother liquor, the method is simpler, easier to control and more liable to large-scale production, lowers production cost and overcomes the shortages that the traditional method for producing the dehydropregnenolone acetate recycles the mother liquor and causes the low yield rate and poor quality of the product; simultaneously, the method obtains high-purity dehydropregnenolone acetate with content over 99 percent and melting point over 169 DEG C.

Description

technical field [0001] The invention belongs to the technical field of production of steroid hormone intermediates, and in particular relates to a production method of high-purity dienolone acetate. Background technique [0002] The chemical name of dienolone acetate (referred to as diene) is: 5,16-pregnadiene-3β-ol-20-one acetate, and the molecular formula is C 23 h 32 o 3 . It is an important intermediate for the synthesis of steroid hormone APIs, and it can be used as a raw material to produce adrenal hormone drugs (such as cortisone), glucocorticoid drugs, steroidal anti-inflammatory drugs (such as dexamethasone acetate, peptide Easy) and sex hormone drugs (such as progesterone) and oral contraceptives for women. At present, the industrial production of dienolone acetate is mainly semi-synthesized from steroids isolated from natural resources. The raw materials for the synthesis of dienolone acetate mainly include diosgenin, sisal saponin, and saponin in steroidal s...

AI Technical Summary

Problems solved by technology

At present, most manufacturers mainly use the mother liquor to extract the hydrolyzed product with n-hexane or cyclohexane to obtain the crude product of dienolone acetate and the mother liquor. The crude product is heated and recrystallized with ethanol to obtain the high-quality product. The dienolone acetate product, part of the unreacted saponin, and the low-polarity impurities in the above three-step reaction process all remain in the mother liquor, and the mother liquor is put into the ring-opening kettle. On the one hand, this treatment method The quality of the dienolone acetate product obtained is not high, and the general melting point is above 165 ° C; on the other hand, a considerable part of the dienolone acetate product with low content and some unreacted saponin, and the above three-step reaction process The low-polarity impurities of low-polarity impurities are all left in the mother liquor, and such recycling increases the difficulty of subsequent processing and the instability of the reaction, which reduces the yield and product quality.

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