Method for producing high purity diene alcohol ketone acetic ester

A dienolone acetate, high-purity technology, applied in the direction of steroids, organic chemistry, etc., can solve the problem of low quality of dienolone acetate, increased difficulty and instability, reduced yield and product quality, etc. problems, to achieve the effect of low equipment requirements, easy operation, and improved production efficiency

Inactive Publication Date: 2009-04-08
HUNAN KEYUAN BIO PRODS
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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, t

Method used

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  • Method for producing high purity diene alcohol ketone acetic ester

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Embodiment 1

[0023] Take 1Kg of diosgenin (melting point above 195°C), crack under pressure, oxidize, and hydrolyze (eliminate), extract the hydrolyzate with cyclohexane, remove the acid water from the cyclohexane extract, wash with water until neutral, and Sedimentation and water separation for 24h. Dilute the above-mentioned cyclohexane to a diene concentration of 2%, wet-pack the silica gel column with cyclohexane, and elute with cyclohexane: ethyl acetate = 20:1, and elute to 2BV. This section is an impurity, mainly Contain discarded. Then elute 4BV, stop collecting, combine this section, concentrate to a small volume, and dry by suction filtration to obtain pure white needle-like crystals with a melting point above 169°C and 650g of dienolone acetate fine product with a content of more than 99%. The rate is 65%. The adsorption layer of the silica gel column is dug out, extracted with methanol, and the concentrated extract is recycled and put into the open-loop kettle.

Embodiment 2

[0025] Get dienolone acetate crude product 10g (more than 165 ℃ of fusing points, content 98%), carry out dissolving with normal hexane to concentration containing diene concentration at 1%, with normal hexane wet packing silica gel column, with normal hexane: chloroform = 9:1 ​​for elution, elution to 3BV, this section is a low polarity impurity. Then elute 5BV, stop collecting, combine this section, concentrate to a small volume, and dry by suction filtration to obtain pure white needle-like crystals, 9.6g of dienolone acetate refined product with a melting point above 169°C and a content of more than 99%.

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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...

Claims

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Application Information

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IPC IPC(8): C07J7/00
Inventor 刘志强
Owner HUNAN KEYUAN BIO PRODS
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