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Method for manufacturing dehydropregnenolone acetate by using mixed solvent

A technology of dienol ketone acetate and mixed solvent, which is applied in the production field of intermediates, can solve the problems of long time consumption, complicated operation process and high production cost, and achieve the goal of short time consumption, high purity and low production cost Effect

Inactive Publication Date: 2013-04-17
湖北省丹江口开泰激素有限责任公司 +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Aiming at the problems of complex operation process, long time consumption and high production cost in the above technologies, the present invention provides a method for producing gestational dienol ketone acetate with mixed solvents, which is simple in operation, short in time and low in production cost.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] The synthetic technique of the thick product of dienol ketone ester of acetic acid pregnancy belongs to mature technology in the prior art, and the synthetic technique of the thick product of dienol ketone ester of acetic acid pregnancy that the present invention adopts preferably following method:

[0062] The method takes diosgenin as raw material, and carries out the following steps successively:

[0063] Ring-opening: Under stirring conditions, add diosgenin to the mixed solution composed of acetic anhydride and glacial acetic acid to react to obtain the ring-opened mixed solution. The reaction pressure is below -0.07MPa, the temperature is 192-210°C, and the reaction time 40-50 minutes, the mass ratio of diosgenin, glacial acetic acid and acetic anhydride is 1:0.5-1.5:0.8-1.9, the mass percentage concentration of glacial acetic acid is ≥98%, and the mass percentage concentration of acetic anhydride is ≥98%;

[0064] Oxidation: add chromium trioxide, sodium acetate,...

Embodiment 2

[0073] The steps are the same as in Example 1, except that the volume ratio of dichloromethane to alcohols is 1:3.6. The yield of the finally obtained pregnancy dienol ketone acetate product is 67.0%, and the purity is 99.4%.

Embodiment 3

[0075] The steps are the same as in Example 1, except that the volume ratio of dichloromethane to alcohols is 1:4. The yield of the finally obtained pregnancy dienol ketone acetate product is 68.0%, and the purity is 99.5%.

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Abstract

The invention provides a method for manufacturing dehydropregnenolone acetate by using a mixed solvent. In the method, with diosgenin as a raw material, the dehydropregnenolone acetate is obtained through open-loop, oxidation, hydrolysis, extraction and concentration as well as refining processes; and the refining process comprises a heating and refluxing step and a cooling and recrystallizing step, as well as a separating and drying step. According to the invention, as the mixed solvent formed by dichloromethane and alcohols replaces the traditional ethanol solvent to refine a dehydropregnenolone acetate crude product, the dehydropregnenolone acetate product with high purity, high yield and excellent appearance is obtained; in addition, in the refining process, the adding of an ethanol washing step is also beneficial for increasing the purity of the dehydropregnenolone acetate product; and the method for manufacturing the dehydropregnenolone acetate by using the mixed solvent, provided by the invention, has the advantages of simplicity in operation, short time and low production cost and is easy for large-scale industrial production.

Description

technical field [0001] The invention belongs to the technical field of production of intermediates of steroid hormone drugs, and in particular relates to a method for producing gestational dienol ketone acetate with a mixed solvent. Background technique [0002] The chemical name of Pregnant Dienol Ketone Acetate is 3β-hydroxy-pregna-5(6),16(17)-dien-20-one acetate and the molecular formula is C 23 h 32 o 3 , a typical steroid compound. Pregnancy dienol ketone acetate is an important intermediate in the synthesis of steroid hormone drugs, and it can be used as raw materials to produce steroidal anti-inflammatory drugs, contraceptives and sex hormone drugs. At present, the industrial production of pregnant dienol ketone acetate is mainly semi-synthesized from steroids isolated from natural resources, and diosgenin is the main raw material for the synthesis of pregnant dienol ketone acetate. As a big producer of diosgenin, most of the techniques for producing acetic acid g...

Claims

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Application Information

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IPC IPC(8): C07J13/00
Inventor 闻开学池汝安曹雪山张越非李勇余军霞徐志高肖春桥张美
Owner 湖北省丹江口开泰激素有限责任公司
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