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A kind of refining method of halometasone

A purification method and a halometasone technology, applied in the directions of steroids, organic chemistry, etc., can solve the problems of low purification yield, complicated operation, etc., and achieve the effects of high yield, simple and easy method, and low cost.

Active Publication Date: 2016-09-14
HUNAN MINGRUI PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Experiments show that this method has a low refining yield and is cumbersome to operate

Method used

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  • A kind of refining method of halometasone
  • A kind of refining method of halometasone
  • A kind of refining method of halometasone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Embodiment 1: Halometasone is refined

[0034] Take 5.0g of halometasone crude product and add it to a 500ml reaction bottle, add 20ml of methanol into it, stir to dissolve it, after it dissolves, add 40ml of purified water into it, immediately a white solid precipitates, continue to stir and crystallize for 2h, filter, 45 After vacuum drying at ℃ for 12 hours, 4.7 g of off-white solid powder was obtained, that is, the refined halometasone product I, with a yield of 94.0%.

Embodiment 2

[0035] Embodiment 2: Refining of Halometasone

[0036] Take 5.0g of halometasone crude product and add it to a 500ml reaction bottle, add 30ml of methanol into it, stir to dissolve it, after it dissolves, add 40ml of purified water into it, immediately a white solid precipitates out, continue to stir and crystallize for 2h, filter, 45 After vacuum drying at ℃ for 12 hours, 4.6 g of off-white solid powder was obtained, that is, the refined halometasone product I, with a yield of 92.0%.

Embodiment 3

[0037] Embodiment 3: Halometasone refining

[0038] Take 5.0g of halometasone crude product and add it to a 500ml reaction bottle, add 40ml of methanol into it, stir to dissolve it, after it dissolves, add 40ml of purified water into it, immediately a white solid precipitates, continue to stir and crystallize for 2h, filter, 45 After vacuum drying at ℃ for 12 hours, 4.6 g of off-white solid powder was obtained, that is, the refined halometasone product I, with a yield of 92.0%.

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Abstract

The invention relates to a method for refining halomethasone monohydrate. The method comprises the following steps: dissolving halomethasone monohydrate in methanol, then adding purified water, stirring for crystallization, filtering, and drying to obtain a refined halomethasone monohydrate product I; and dissolving the refined halomethasone monohydrate product I in ethyl acetate, then adding normal heptane, stirring for cooling crystallization, filtering, washing normal heptane, and drying to obtain halomethasone monohydrate. According to the method, although refining is carried out twice, an obtained product has high product purity (the single unknown impurity content is lower than and equal to 0.1%), and produced halomethasone monohydrate accords with the national and international crude drug quality standards.

Description

technical field [0001] The invention relates to a method for refining halometasone. Background technique [0002] Halometasone [0003] [0004] Halometasone, as a skin disease that responds to adrenocortical hormones for external use, has rapid anti-inflammatory, anti-allergic, anti-itching, anti-exudation and anti-proliferation effects, with strong activity and fast action. [0005] In the process of synthesizing halometasone, various impurities are inevitably produced, which are difficult to remove. [0006] Patent document US3652554 has reported the synthetic and refining method of halometasone, and it adopts the chlorination of flumetasone ethyl ester to generate diclomethasone ethyl ester, and diclomethasone ethyl ester generates monoclomethasone ethyl ester through pyridine dechlorination, and then monochloride Flumetasone ethyl ester is hydrolyzed by sodium bicarbonate aqueous solution to generate halometasone crude product, and through silica gel column chromat...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J5/00
CPCC07J5/0076
Inventor 蔡辉刘爱民易申赢叶凯
Owner HUNAN MINGRUI PHARMA