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Preparation method and preparation system of medroxyprogesterone acetate

A technology of medroxyprogesterone acetate and acetic acid, which is applied in the field of preparation methods and systems of medroxyprogesterone acetate, can solve the problems of inability to realize large-scale production and high cost of raw materials, achieve convenient separation and collection, ensure purity, reduce original cost effect

Active Publication Date: 2017-06-20
YUEYANG HUANYU PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Most of the existing preparations of medroxyprogesterone acetate are made of complex ketones through chemical reactions, and the cost of raw materials is high, so large-scale production cannot be realized

Method used

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  • Preparation method and preparation system of medroxyprogesterone acetate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] A preparation method of medroxyprogesterone acetate, it comprises the steps:

[0027] ①. Preparation of methine acetate, pump 450 parts of tetrahydrofuran into the reaction kettle, add 150 parts of monoester, stir, pump in 60 parts of triethyl orthoformate, 80 parts of absolute ethanol, blow nitrogen, add 1.5 parts of PTS for decolorization Reaction at 34°C for 1 hour, then add 1.5 parts of PTS decolorizer, and react for 1.5 hours; lower the above reaction solution to 28°C, sequentially pump in 45 parts of N-methylaniline and 45 parts of formaldehyde, and heat up to 36°C React for 2.5 hours, pump the reaction liquid into the water analysis kettle, cool down to 15°C, add 180 parts of hydrochloric acid dropwise for 30 minutes, then keep it at 23°C for 1.5 hours, add 1800 parts of drinking water for water analysis, cool down to 5°C, and stir for 3 hours , centrifuged, added 300 parts of water to wash until neutral, and dried to obtain 150 parts of methine acetate, 50 parts...

Embodiment 2

[0031] A preparation method of medroxyprogesterone acetate, it comprises the steps:

[0032] ①. Preparation of methine acetate, pump 450 parts of tetrahydrofuran into the reaction kettle, add 150 parts of monoester, stir, pump in 60 parts of triethyl orthoformate, 80 parts of absolute ethanol, blow nitrogen, add 1.5 parts of PTS for decolorization Add 1.5 parts of PTS decolorizing agent and react for 1.5 hours; lower the above reaction solution to 28 ℃, sequentially pump in 45 parts of N-methylaniline and 45 parts of formaldehyde, and heat up to 34 ℃ React for 2.5 hours, pump the reaction liquid into the water analysis kettle, cool down to 15°C, add 180 parts of hydrochloric acid dropwise for 30 minutes, then keep it at 27°C for 1.5 hours, add 1800 parts of drinking water for water analysis, cool down to 5°C, and stir for 3 hours , centrifuged, added 300 parts of water to wash until neutral, and dried to obtain 150 parts of methine acetate, 50 parts of water vapor and 2613 par...

Embodiment 3

[0036] A preparation method of medroxyprogesterone acetate, it comprises the steps:

[0037] ①. Preparation of methine acetate, pump 450 parts of tetrahydrofuran into the reaction kettle, add 150 parts of monoester, stir, pump in 60 parts of triethyl orthoformate, 80 parts of absolute ethanol, blow nitrogen, add 1.5 parts of PTS for decolorization Reaction at 35°C for 1 hour, then add 1.5 parts of PTS decolorizing agent, and react for 1.5 hours; lower the above reaction solution to 28°C, sequentially pump in 45 parts of N-methylaniline and 45 parts of formaldehyde, and heat up to 35°C React for 2.5 hours, pump the reaction liquid into the water analysis kettle, cool down to 15°C, add 180 parts of hydrochloric acid dropwise for 30 minutes, then keep it at 25°C for 1.5 hours, add 1800 parts of drinking water for water analysis, cool down to 5°C, and stir for 3 hours , centrifuged, added 300 parts of water to wash until neutral, and dried to obtain 150 parts of methine acetate, 5...

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Abstract

The invention relates to the field of preparation of medicines and in particular relates to a preparation method of medroxyprogesterone acetate. The preparation method comprises the steps of methenyl acetate preparation, hydrogenation reaction, de-coloring and refining and the like; the invention further provides a preparation system of the medroxyprogesterone acetate; the preparation system comprises a methenyl acetate preparation mechanism, a hydrogenation reaction mechanism and a de-coloring and refining mechanism, which are connected in sequence; the invention aims at providing the preparation method and the preparation system of the medroxyprogesterone acetate; a monoester is used as a raw material and reacts to prepare methenyl acetate; then the hydrogenation reaction and de-coloring and refining reaction are carried out to prepare the medroxyprogesterone acetate; the monoester is simple and easy to obtain, so that the cost of the raw material can be reduced; a preparation process is stable and the obtained medroxyprogesterone acetate has high purity; the preparation method can be adaptive to large-scale production.

Description

technical field [0001] The invention relates to the field of medicine preparation, in particular to a preparation method and a preparation system of medroxyprogesterone acetate. Background technique [0002] Medroxyprogesterone acetate is a commonly used medicine, mainly used for dysmenorrhea, functional amenorrhea, functional uterine bleeding, threatened abortion or habitual abortion, endometriosis, treatment of advanced breast cancer, endometrial gland cancer and kidney cancer. Large doses can be used as long-acting contraceptive injections. In addition, the effect is also reflected in the menstrual cramps due to the loss of estrogen and progesterone support in the endometrium, and can continue to artificially supplement estrogen or progesterone, especially progesterone, so that the "helpless" endometrium continues to prosper. Get support and maintain the level of continued thickening, so that the endometrium grows firmly on the uterine wall, making preparations for the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J7/00
CPCC07J7/0045
Inventor 徐润星
Owner YUEYANG HUANYU PHARMA
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