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Preparation method of 17beta-cyano-17alpha-hydroxypregna-4-ene-3-one

A hydroxypregnant and cyano technology, which is applied in the field of preparation of 17β-cyano-17α-hydroxypregn-4-en-3-one, can solve the problems of long reaction time and inability to treat cyanide-containing wastewater, and achieves the reaction The effect of short time, yield and quality improvement

Pending Publication Date: 2021-12-14
佳尔科生物科技南通有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] However, the 17β-cyano-17α-hydroxypregn-4-en-3-one preparation process involved in the above-mentioned disclosed documents all has a long reaction time, usually more than 15h, and a large amount of cyanide-containing wastewater is produced during the production process. Dealing with the problem

Method used

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  • Preparation method of 17beta-cyano-17alpha-hydroxypregna-4-ene-3-one
  • Preparation method of 17beta-cyano-17alpha-hydroxypregna-4-ene-3-one

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Experimental program
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Embodiment 1

[0027] Add 200kg of 4-AD and 2000kg of methanol into the autoclave, add 0.2kg of sodium hydroxide as a catalyst, and slowly add 20kg of hydrocyanic acid dropwise; react at 80°C and 1.5Mpa for 2 hours; use HPLC tracking analysis, the raw material content is less than 0.5 %, the reaction is ended; after cooling, the material enters a device integrated with filtration, washing, drying and discharging to obtain 17β-cyano-17α-hydroxypregnene-4-ene- 214kg of 3-ketone, weight yield 107%.

[0028] The mother liquor after the above reaction can be directly recovered and used mechanically without other treatment.

Embodiment 2

[0030] Add 200kg of 4-AD and 600kg of ethanol to the autoclave, add 5kg of sodium hydroxide, and slowly add 20kg of hydrocyanic acid dropwise; react at 30°C and 1Mpa for 3 hours; HPLC tracking analysis, when the raw material content is less than 0.5%, the reaction is terminated After cooling, the material enters the integrated device of filtration, washing, drying and discharging, and obtains 215kg of 17β-cyano-17α-hydroxyl pregn-4-en-3-one with a content of 98.6% (HPLC normalization method). The weight yield was 107.5%.

[0031] The mother liquor after the above reaction can be directly recovered and used mechanically without other treatment.

Embodiment 3

[0033] Add 200kg of 4-AD and 1400kg of ethanol to the autoclave, add 10kg of sodium hydroxide, and slowly add 20kg of hydrocyanic acid dropwise; react at 55°C and 0.1Mpa for 3 hours; follow-up analysis by HPLC, when the raw material content is less than 0.5%, the end Reaction; after cooling, the material enters a device integrated with filtration, washing, drying and discharge to obtain 215kg of 17β-cyano-17α-hydroxypregna-4-en-3-one with a content of 98.6% (HPLC normalization method) , The weight yield is 107.5%.

[0034] The mother liquor after the above reaction can be directly recovered and used mechanically without other treatment.

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Abstract

The invention discloses a preparation method of 17beta-cyano-17alpha-hydroxypregna-4-ene-3-one. The preparation method comprises the following step: reacting hydrocyanic acid serving as a cyaniding agent with 4-AD in the presence of a basic catalyst, so as to prepare the 17beta-cyano-17alpha-hydroxypregna-4-ene-3-one. The whole reaction is a totally-closed system, and a device integrating filtering, washing, drying and discharging is adopted for post-treatment of the product. Excessive hydrocyanic acid is directly recycled and reused in the mother liquor, no environmental problem is generated, the reaction time is short, and the yield and the purity are both improved.

Description

technical field [0001] The invention belongs to the technical field of steroid drugs and chemical industry, and relates to a preparation method of 17β-cyano-17α-hydroxypregn-4-en-3-one. Background technique [0002] 17α-hydroxyprogesterone is also known as 17α-hydroxypregn-4-ene-3,20-dione, molecular formula: C 21 h 30 o 3 , Density: 1.15g / cm 3 , which is a white diamond-shaped or hexagonal leaflet-shaped crystal, is an endogenous progesterone, which can be produced by the human body itself, and there are also chemical preparations. It is a long-acting progestogen, its progesterone activity is 7 times that of progesterone, and it has no estrogen activity. [0003] 17β-cyano-17α-hydroxypregn-4-en-3-one is an important intermediate in the synthesis of 17α-hydroxyprogesterone. Li Xingtai et al. published documents, patent publications CN104072565A, CN201310107890.1 and CN201410331816.2, etc. disclose the synthesis of 17β-cyano-17α-hydroxypregna-4-ene-3 by using 4-AD as raw...

Claims

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Application Information

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IPC IPC(8): C07J3/00
CPCC07J3/005
Inventor 王彩霞周革
Owner 佳尔科生物科技南通有限公司