Preparation method of medroxyprogesterone acetate for perimenopausal syndrome

A technology of medroxyprogesterone acetate and ketone acetate, applied in the field of medicine and chemical industry, can solve the problems of long time, many reaction steps, low yield and the like, and achieves the effects of low cost, less raw material usage and high yield

Active Publication Date: 2022-02-18
HEILONGJIANG UNIV OF CHINESE MEDICINE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0016] It can be seen that the existing preparation method of medroxyprogestero...

Method used

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  • Preparation method of medroxyprogesterone acetate for perimenopausal syndrome
  • Preparation method of medroxyprogesterone acetate for perimenopausal syndrome
  • Preparation method of medroxyprogesterone acetate for perimenopausal syndrome

Examples

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Embodiment 1

[0052] In a reactor equipped with a reflux condenser, a dropping funnel, and a magnetic stirring device, add sodium acetate (3.0 g), aluminum trichloride (266 mg, 2 mmol), 1,3-dioxane (12 ml, about 12.8 g), then added anhydrous chloroform (200ml) and stirred at reflux for 0.5h. Subsequently, 17α-hydroxyprogesterone acetate (3.73g, 10mmol) was added and stirred to dissolve to form a reaction solution, then phosphorus oxychloride (2.8ml, 30mmol) was slowly added dropwise to the reaction solution through a dropping funnel, 1.5 h is added. After the addition, continue to stir the reaction under reflux for 3h. The reaction solution was naturally cooled to room temperature, then a saturated aqueous sodium carbonate solution was added dropwise under vigorous stirring to quench the reaction, the pH of the aqueous layer was monitored, and the addition of a saturated aqueous sodium carbonate solution was stopped when it reached alkalinity (pH was 7-8); Remove the insoluble matter by f...

Embodiment 2

[0054] In a reactor equipped with a reflux condenser, dropping funnel, and magnetic stirring device, add sodium acetate (3.0 g), aluminum trichloride (200 mg, 1.5 mmol), 1,3-dioxane (12 ml, about 13g), then added anhydrous chloroform (200ml) and stirred at reflux for 0.5h. Subsequently, 17α-hydroxyprogesterone acetate (3.73g, 10mmol) was added and stirred to dissolve to form a reaction solution, then phosphorus oxychloride (2.8ml, 30mmol) was slowly added dropwise to the reaction solution through a dropping funnel, 1.5 h is added. After the addition was complete, the stirring reaction was continued under reflux for 3.5h. The reaction solution was naturally cooled to room temperature, then a saturated aqueous sodium carbonate solution was added dropwise under vigorous stirring to quench the reaction, the pH of the aqueous layer was monitored, and the addition of a saturated aqueous sodium carbonate solution was stopped when it reached alkalinity (pH was 7-8); Remove the insol...

Embodiment 3

[0056] In a reactor equipped with a reflux condenser, dropping funnel, and magnetic stirring device, add sodium acetate (3.0 g), aluminum trichloride (200 mg, 1.5 mmol), 1,3-dioxane (15 ml, about 16g), then added anhydrous chloroform (200ml) and stirred at reflux for 0.5h. Subsequently, 17α-hydroxyprogesterone acetate (3.73g, 10mmol) was added and stirred to dissolve to form a reaction solution, then phosphorus oxychloride (2.3ml, 25mmol) was slowly added dropwise to the reaction solution through the dropping funnel, 1.5 h is added. After the addition was complete, the stirring reaction was continued under reflux for 3.5h. The reaction solution was naturally cooled to room temperature, then a saturated aqueous sodium carbonate solution was added dropwise under vigorous stirring to quench the reaction, the pH of the aqueous layer was monitored, and the addition of a saturated aqueous sodium carbonate solution was stopped when it reached alkalinity (pH was 7-8); Remove the ins...

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Abstract

The invention relates to a preparation method of medroxyprogesterone acetate for perimenopausal syndrome. Compared with the prior art, the preparation method disclosed by the invention has the advantages of few steps, simplicity in operation, short total reaction time, high yield, less raw material consumption, low cost, good product quality and the like. The preparation method of medroxyprogesterone acetate has high economic value and is suitable for industrial application.

Description

technical field [0001] The invention relates to the field of medicine and chemical industry, in particular, the invention relates to a preparation method of medroxyprogesterone acetate for perimenopausal syndrome. Background technique [0002] Medroxyprogesterone 17-acetate, also known as medroxyprogesterone acetate, medroxyprogesterone, medroxyprogesterone, etc., chemical name is 17α-hydroxy-6α-methylpregna-4-ene-3, 20-diketone acetate, developed by Upjohn Company of the United States, has a trade name of Provera. Medroxyprogesterone acetate is a new type of lutein progesterone drug, which can be widely used clinically in the treatment of perimenopausal syndrome, dysmenorrhea, irregular menstruation, dysfunctional uterine bleeding, threatened abortion and endometriosis It is widely used in clinical practice, and the market demand continues to rise. [0003] The synthetic routes of medroxyprogesterone acetate mainly contain the following types: [0004] Route 1 (Liisberg ...

Claims

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Application Information

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IPC IPC(8): C07J7/00
CPCC07J7/0045C07B2200/07
Inventor 张跃辉吴效科姜玥张蛟
Owner HEILONGJIANG UNIV OF CHINESE MEDICINE
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