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Preparation method of betamethasone intermediate

A technology for betamethasone and intermediates, which is applied in the field of preparation of betamethasone intermediates, can solve problems such as low yield and side chain degradation, and achieve the effects of high yield, good quality, and good industrial production value

Inactive Publication Date: 2014-04-16
SHANGHAI NEW HUALIAN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Its shortcoming is that in the hydrolysis reaction process, the product easily causes the degradation of the side chain in the strong alkaline solution, so the yield of the prior art is on the low side, only about 82%

Method used

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  • Preparation method of betamethasone intermediate
  • Preparation method of betamethasone intermediate
  • Preparation method of betamethasone intermediate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Add 20g of betamethasone replacement (II) into a 1000ml three-necked bottle, add 600ml of methanol and 120ml of dichloromethane, heat up to reflux, reflux for 15 minutes, add dropwise 30ml of 20% sodium sulfite solution for hydrolysis reaction, after the reaction is complete, use glacial acetic acid Neutralize to pH=6.5, concentrate the reaction solution under reduced pressure at 40°C to 50°C to near dryness, pour into tap water for water analysis, filter, wash the filter cake with water, dry to obtain 17.5g of betamethasone hydrolyzate (I), and detect by HPLC The content is 98.2%.

Embodiment 2

[0023] Add 20g of betamethasone replacement (II) into a 1000ml three-neck flask, add 800ml of methanol and 100ml of dichloromethane, heat up to reflux, reflux for 15 minutes, add 40ml of 20% sodium sulfite solution dropwise for hydrolysis reaction, after the reaction is complete, use glacial acetic acid Neutralize to pH=6.5, concentrate the reaction solution under reduced pressure at 40°C to 50°C to nearly dryness, pour into tap water for water analysis, filter, wash the filter cake with water, dry to obtain 17.6g of betamethasone hydrolyzate (I), and detect by HPLC The content is 97.8%.

Embodiment 3

[0025] Add 20g of betamethasone replacement (II) into a 1000ml three-necked bottle, add 700ml of methanol and 100ml of dichloromethane, heat up to reflux, reflux for 15 minutes, add 50ml of 20% sodium sulfite solution dropwise for hydrolysis reaction, after the reaction is complete, use glacial acetic acid Neutralize to pH=6.5, concentrate the reaction solution under reduced pressure at 40°C to 50°C to near dryness, pour into tap water for water analysis, filter, wash the filter cake with water, dry to obtain 17.4g of betamethasone hydrolyzate (I), and detect by HPLC The content is 98.4%.

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Abstract

The invention discloses a preparation method of betamethasone intermediate hydrolysate (I), which employs a betamethasone substitute (II) as substrate, and employs a hydrolytic agent with reductibility to hydrolyze, and a compound in formula (I) is obtained. The reaction formula is shown in the figure. The invention employs the hydrolytic agent with reductibility to prepare the hydrolysate (I), and has the characteristics of high yield and good quality with good industrial production value.

Description

technical field [0001] The invention belongs to the field of organic synthesis chemistry, and in particular relates to a preparation method of a betamethasone intermediate. Background technique [0002] Betamethasone is an important and potent glucocorticoid. The traditional method for preparing betamethasone intermediate hydrolyzate (I) compound is to use the compound of formula (II) as the substrate, dissolve the substrate in an organic solvent, dissolve the Then add sodium hydroxide or potassium hydroxide to carry out hydrolysis reaction. After the reaction is completed, neutralize with glacial acetic acid. The reaction solution is concentrated to dryness under reduced pressure, flushed with water for water analysis, and dried to obtain the hydrolyzate (I). The reaction equation is as follows: [0003] [0004] Its shortcoming is that in the hydrolysis reaction process, the product easily causes the degradation of the side chain in the strong alkaline solution, so the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J71/00
Inventor 潘高峰贺一君徐志超卿文彬吴庆安周福群周秋火
Owner SHANGHAI NEW HUALIAN PHARMA
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