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Fluorous synthesis method of betamethasone

A technology of betamethasone and synthetic methods, applied in the direction of steroids, organic chemistry, etc.

Inactive Publication Date: 2012-01-04
ZHEJIANG XIANJU XIANLE PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The functional groups on the drug structure interfere with each other, so the chemical reaction is very complicated
It is manifested in the complex synthetic process route, many chemical reaction steps, low utilization rate of raw materials, large amount of auxiliary materials, long production cycle, many side reactions, many solvents used in the reaction process, more waste water and waste gas, and difficult recycling. , low economic and technical indicators, high cost, etc., such as the following synthetic method
Moreover, the foreign production process is basically similar to the domestic process, and there are also the same problems

Method used

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  • Fluorous synthesis method of betamethasone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Pour 50g of hydrogen fluoride into 24g of water, cool down to -30°C, then slowly add 20g of betamethasone epoxy, and control the internal temperature of the fluorine reaction at -20°C, after the reaction is complete, cool the feed solution to -30°C ℃, standby;

[0036] Take the feed solution obtained above and heat it up to 20°C, then add 100g of sodium carbonate and 400ml of aqueous solution for water analysis, and filter the precipitated products in turn, flush with water until neutral, and dry to obtain a wet product of fluoride on betamethasone;

[0037] Put the wet product of betamethasone fluoride into 400ml of methanol, add 4g of activated carbon to reflux for 30 minutes, filter, concentrate to 40ml mother liquor, cool to 10°C and filter to obtain the wet product of betamethasone.

[0038] Get the wet product of betamethasone obtained above and dry it at 55° C. for 2 hours to obtain 17.2 g of betamethasone.

[0039] Embodiment 1 The yield of betamethasone is 86%...

Embodiment 2

[0041] Pour 36g of hydrogen fluoride into 30g of water, cool down to -32°C, then slowly add 20g of betamethasone epoxy, and control the internal temperature of the fluorine reaction at -20°C, after the reaction is complete, cool the feed solution to -32°C ℃, standby;

[0042] Take the feed liquid obtained above and heat it up to 25°C, then add 125g of sodium carbonate and 375ml of aqueous solution for water analysis, and filter the precipitated products in turn, flush with water until neutral, and dry to obtain a wet product of fluoride on betamethasone;

[0043] Put the wet product of betamethasone fluoride into 400ml of methanol, add 4g of activated carbon to reflux for 30 minutes, filter, concentrate to 40ml mother liquor, cool to 10°C and filter to obtain the wet product of betamethasone.

[0044] Get the wet product of betamethasone obtained above and dry at 60° C. for 3 hours to obtain 17.2 g of betamethasone.

[0045] Embodiment 2 The yield of betamethasone is 87%, and...

Embodiment 3

[0047] Pour 36g of hydrogen fluoride into 24g of water, cool down to -34°C, then slowly add 20g of betamethasone epoxy, and control the internal temperature of the fluorine reaction to -10°C, after the reaction is complete, cool the feed solution to -35°C ℃, standby;

[0048] Take the feed solution obtained above and heat it up to 30°C, then add 75g of sodium carbonate and 425ml of aqueous solution for water analysis, and filter the precipitated products in turn, flush with water until neutral, and dry to obtain a wet product of fluoride on betamethasone;

[0049] Put the wet product of betamethasone fluoride into 400ml of methanol, add 4g of activated carbon to reflux for 30 minutes, filter, concentrate to 40ml mother liquor, cool to 10°C and filter to obtain the wet product of betamethasone.

[0050] Get the wet product of betamethasone obtained above and dry it at 58° C. for 4 hours to obtain 17.4 g of betamethasone.

[0051]Embodiment 3 The yield of betamethasone is 87%, ...

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Abstract

The invention relates to a fluorous synthesis method of betamethasone, belonging to the technical field of steride medicament synthesis methods in pharmaceutical chemistry. The method comprises the following process steps: fluorinating and refining betamethasone epoxide which is used as a raw material so as to obtain betamethasone. According to the invention, the fluorous synthesis method of betamethasone is reasonable in design, thus chemical reaction time is greatly reduced, production period is shortened, a whole technical level of a product is greatly improved, cost is reduced by 15% as compared with the conventional process, and the fluorous yield of betamethasone reaches 85-90%.

Description

technical field [0001] The invention belongs to the technical field of steroid drug synthesis methods in medicinal chemistry, and in particular relates to a method for synthesizing fluorine on betamethasone. Background technique [0002] Betamethasone, its structural formula (Formula (1)), is a high-efficiency halogen-containing corticosteroid drug, which acts on glucose metabolism, can reduce the pathological changes of the body tissue to damaging stimuli, and has high curative effect and small side effects. It can treat Lupus erythematosus, rheumatoid arthritis, asthma and other serious diseases are widely used in international clinics. Since it was successfully developed in the 1970s in the world, its market sales have been very popular, ranking first in hormones. There are only a dozen domestic companies in normal production, and the yield of fluorine synthesis is only 75%. [0003] [0004] Formula 1). [0005] The process route for producing synthetic betamethaso...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J5/00
Inventor 张和明
Owner ZHEJIANG XIANJU XIANLE PHARMA
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