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Production process method of 16, 17 doublebond steroidal pharmaceutical intermediate

A process method and technology of production process, applied in the field of production process of 16,17 double-bond steroid drug intermediates, can solve problems such as safety is not easy to guarantee, many reaction steps, environmental pollution, etc., and achieve favorable reaction yield and The effect of product quality, mild reaction conditions and shortened process route

Inactive Publication Date: 2010-06-30
TIANJIN JINYAO GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The traditional method for preparing 16,17-double bond intermediate (I) needs to go through three steps of chemical reaction, with 16,17 epoxy intermediate (II) as raw material, through bromohydryl ring opening, debromination, dehydration reaction, reaction There are many steps, the yield of the product obtained is low, and there are many by-products, and nickel-catalyzed hydrogenation debromination is used in the debromination reaction, and SOx is required for the dehydration reaction. 2 , POCl 3 And other reagents, hydrogenation reaction needs to use highly flammable and explosive hydrogen, safety is not easy to guarantee, and POCl 3 Unstable, and will produce irritating HCl gas, serious environmental pollution

Method used

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  • Production process method of 16, 17 doublebond steroidal pharmaceutical intermediate
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  • Production process method of 16, 17 doublebond steroidal pharmaceutical intermediate

Examples

Experimental program
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Effect test

Embodiment 1

[0021] Embodiment 1: the synthesis of compound Ia,

[0022]

[0023] Get compound (IIa) 10g, content 95%, be dissolved in 50ml absolute ethanol, nitrogen protection, add the chromous acetate 0.05mol that dissolves in water under nitrogen protection, carry out reaction, reaction temperature is 10~20 ℃, under nitrogen protection, After the reaction was completed under protection, the reaction solution was diluted with a large amount of water, filtered, and dried to obtain 8.2 g of compound (Ia), with a content of 90.1%.

Embodiment 2

[0024] Embodiment 2: the synthesis of compound Ib

[0025]

[0026] Get compound (IIb) 10g, content 95%, dissolve in 100ml95% ethanol, nitrogen protection, under nitrogen protection, add the chromous chloride soluble in water 0.1mol, carry out reaction, reaction temperature is 20~30 ℃, under nitrogen protection After the reaction was completed under protection, the reaction solution was diluted with a large amount of water, filtered, and dried to obtain 8.1 g of compound (Ib) with a content of 90.5%.

Embodiment 3

[0027] Embodiment 3: the synthesis of compound Ic

[0028]

[0029] Take compound (IIc) 10g, content 95%, dissolve in 150ml95% ethanol, nitrogen protection, under nitrogen protection, add the chromous chloride soluble in water 0.15mol, carry out reaction, reaction temperature is 0~10 ℃, under nitrogen protection After the reaction was complete under protection, the reaction solution was diluted with a large amount of water, filtered, and dried to obtain 8.3 g of compound (Ic), with a content of 91%.

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Abstract

A production process method of a 16, 17 doublebond steroidal pharmaceutical intermediate is characterized by taking 16, 17 epoxy intermediate (II) as raw material, reacting with reducing agent of chromous salt, adopting ethanol as solvent, diluting reaction liquid with large amount of water after the reaction, filtering, drying and obtaining reducer. The process can reduce the reaction step, shortens the process route, and greatly improves the quality and yield of the reducer (I).

Description

Technical field: [0001] The invention relates to a production method of a steroid drug intermediate. Especially the production method of 16,17 double bond steroid drug intermediate. Background technique: [0002] Steroidal glucocorticoids are an important class of drugs. The prior art shows that the introduction of 16α-methyl on the steroidal core can significantly reduce its sodium ion retention (Basics of Steroidal Chemistry, Lin Jiwen, Chemical Industry Press, 1989.9; 149~151), the steroid hormones with 16α-methyl mainly include dexamethasone and so on. [0003] 16,17 double bond intermediate (I) is an important intermediate in the synthesis of steroid drugs with 16α-methyl [0004] The traditional method for preparing 16,17-double bond intermediate (I) needs to go through three steps of chemical reaction, with 16,17 epoxy intermediate (II) as raw material, through bromohydryl ring opening, debromination, dehydration reaction, reaction There are many steps, the yield o...

Claims

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Application Information

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IPC IPC(8): C07J7/00C07J5/00
Inventor 卢彦昌蒋基平周金萍
Owner TIANJIN JINYAO GRP