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A kind of preparation technology of estradiol and preparation system thereof

A preparation process and estradiol technology, applied in steroids, organic chemistry and other directions, can solve problems such as low yield and inability to meet large-scale needs, and achieve the effects of saving material costs, ensuring purity, and facilitating separation and recycling.

Active Publication Date: 2018-05-25
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 estradiol is biologically prepared, that is, extracted from organisms, the yield is low, and it cannot meet the large-scale demand. Therefore, there is an urgent need for a chemical preparation method that can stably prepare estradiol.

Method used

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  • A kind of preparation technology of estradiol and preparation system thereof

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Embodiment 1

[0028] A preparation process of estradiol, which comprises the following steps:

[0029] ①, Ketal reaction, add 150 parts of 1,4-androstenedione, 180 parts of ethylene glycol, 150 parts of triethyl orthoformate and 3 parts of PTS decolorizing agent in the reaction kettle, control the temperature at 15°C, and keep warm for the reaction After 3.5 hours, add 3 parts of triethylamine to adjust the pH to 3.5, add water for water analysis by dropping, centrifuge and wash until neutral, add 900 parts of water in total, and then dry to obtain 35 parts of water vapor , 1189 parts of waste water and 162 parts of ketals;

[0030] ②, aromatization hydrolysis, add the ketal obtained in step ① into the reaction kettle, then add 1620 parts of tetrahydrofuran, 50 parts of biphenyl, 65 parts of diphenylmethane, blow nitrogen, adjust the temperature to 35 °C, and add 8.1 parts Adjust the temperature of the lithium pellets to 50°C and stir for 30 minutes, cool down to 20°C, dropwise add tetrahy...

Embodiment 2

[0035] A preparation process of estradiol, which comprises the following steps:

[0036] ①, Ketal reaction, add 150 parts of 1,4-androstenedione, 180 parts of ethylene glycol, 150 parts of triethyl orthoformate and 3 parts of PTS decolorizing agent in the reaction kettle, control the temperature at 20°C, and keep warm for the reaction After 2.5 hours, add 3 parts of triethylamine to adjust the pH to 4.2, add water for water analysis by dropping, centrifuge and wash until neutral, add 900 parts of water in total, and then dry to obtain 35 parts of water vapor , 1189 parts of waste water and 162 parts of ketals;

[0037]②, aromatization hydrolysis, add the ketal obtained in step ① into the reaction kettle, then add 1620 parts of tetrahydrofuran, 50 parts of biphenyl, 65 parts of diphenylmethane, blow nitrogen, adjust the temperature to 40 °C, and add 8.1 parts Adjust the temperature of the lithium pellets to 40°C and stir for 30 minutes, cool down to 25°C, dropwise add tetrahyd...

Embodiment 3

[0042] A preparation process of estradiol, which comprises the following steps:

[0043] ①, Ketal reaction, add 150 parts of 1,4-androstenedione, 180 parts of ethylene glycol, 150 parts of triethyl orthoformate and 3 parts of PTS decolorizing agent in the reaction kettle, control the temperature at 18°C, and keep warm for the reaction After 3 hours, add 3 parts of triethylamine to adjust the pH to 4, add water for water analysis by dropping, centrifuge and wash to neutrality, the total amount of water added is 900 parts, and then dry to obtain 35 parts of water vapor, 1189 parts of wastewater and 162 parts of ketal;

[0044] ②, aromatization hydrolysis, add the ketal obtained in step ① into the reaction kettle, then add 1620 parts of tetrahydrofuran, 50 parts of biphenyl, 65 parts of diphenylmethane, blow nitrogen, adjust the temperature to 38 ° C, and add 8.1 parts Adjust the temperature of the lithium pellets to 45°C and stir for 30 minutes, cool down to 22°C, dropwise add ...

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Abstract

The invention relates to the field of preparation of medicines and in particular relates to a preparation process of estradiol. The preparation process comprises the following steps: ketol reaction, aromatization hydrolysis, first de-coloring and refining, reduction reaction and second de-coloring and refining; the invention further relates a preparation system of the estradiol; the preparation system comprises a ketol reaction mechanism, an aromatization hydrolysis mechanism, a first de-coloring and refining mechanism, a reduction reaction mechanism and a second de-coloring and refining mechanism; each mechanism comprises a reaction kettle and a centrifugal drying device; the invention aims at providing the preparation process of the estradiol and the preparation system of the estradiol; the estradiol can be stably prepared through the ketol reaction, aromatization hydrolysis reaction, first de-coloring reaction, the reduction reaction and second de-coloring reaction; the purity, color and luster of the estradiol can be ensured and utilization requirements of medicines are met.

Description

technical field [0001] The invention relates to the field of preparation of medicines, in particular to a preparation process of estradiol and a preparation system thereof. Background technique [0002] Estradiol is a commonly used drug, which is an estrogen therapeutic agent absorbed through the skin. Supplement the deficiency of 17-β-estradiol secreted by women's ovaries, and at the same time avoid the side effects caused by oral administration (breast pain, weight gain, high blood pressure, gallstones and abnormal liver function, etc.). Estrogen can prompt cells to synthesize DNA, RNA and various proteins in corresponding tissues. [0003] Most of the existing estradiol is biologically prepared, that is, extracted from organisms, and the yield is low, which cannot meet the large-scale demand. Therefore, there is an urgent need for a chemical preparation method that can stably prepare estradiol. Contents of the invention [0004] The purpose of the present invention is...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J1/00
CPCC07J1/0062
Inventor 徐润星
Owner YUEYANG HUANYU PHARMA