Novel technology for synthesizing epiandrosterone by adopting 4-androstenedione through selective hydrogenation reducing

A technology of androstenedione and epiandrosterone, which is applied in the field of selective reduction and hydrogenation of 4-androstenedione to synthesize epiandrosterone, can solve the problems of low product purity and yield, high raw material consumption, long reaction route, etc. problems, to achieve the effects of high product purity and yield, shortened reaction routes, and cost savings

Inactive Publication Date: 2016-07-27
湖北省丹江口开泰激素有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The above synthesis process has a longer reaction route and more side reactions, res

Method used

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  • Novel technology for synthesizing epiandrosterone by adopting 4-androstenedione through selective hydrogenation reducing

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] S1, dissolve 100g of 4-androstenedione in 1.2kg of toluene, heat to dissolve, then cool down to 90°C, add 12.5g of titanium dioxide powder, 37.5g of palladium-calcium catalyst, react for 3 hours, take samples for TLC spot detection until the reaction is complete;

[0025] S2, inject hydrogen gas under 1MP pressure, continue to react for 8 hours, take samples for TLC detection until the reaction is completed;

[0026] S3, after the reaction is completed, filter, recycle titanium dioxide powder and metal platinum, remove toluene by distillation, and dry at 65° C. to obtain crude epiandrosterone;

[0027] S4, take 95 g of the crude epiandrosterone obtained in step S3, dissolve it in 3 times the mass of methanol, add 0.02 times the mass of activated carbon, reflux at 60-70°C for 1 hour, suction filter and concentrate to a paste at 50-55°C, and pump The filtered methanol is recycled, cooled and crystallized at 0°C, and the crystals are filtered and dried to obtain the fine e...

Embodiment 2

[0030] S1, dissolve 100g of 4-androstenedione in 1.2kg of toluene, heat to dissolve, then cool down to 100°C, add 0.5g of titanium dioxide powder, 1g of metal platinum, react for 3 hours, take samples for TLC spot detection until the reaction is complete;

[0031] S2, inject hydrogen gas under 2MP pressure, continue to react for 8 hours, take samples for TLC detection until the reaction is completed;

[0032] S3, after the reaction is completed, filter, recycle titanium dioxide powder and metal platinum, remove toluene by distillation, and dry at 65° C. to obtain crude epiandrosterone;

[0033] S4, taking 95 g of the crude epiandrosterone obtained in step S3, dissolving it in 3 times the mass of methanol, adding 0.02 times the mass of activated carbon, refluxing at 60-70°C for 1.5h, suctioning and concentrating to a paste at 50-55°C, The methanol filtered out by suction is recycled, cooled and crystallized at 5°C, and the crystals are filtered and dried by suction to obtain th...

Embodiment 3

[0037] S1, dissolve 100g of 4-androstenedione in 1.2kg of toluene, heat to dissolve, then cool down to 100°C, add 20g of titanium dioxide powder, 80g of palladium carbon catalyst, react for 5h, take samples for TLC spot detection until the reaction is complete;

[0038] S2, introduce hydrogen gas under 2MP pressure, continue to react for 10h, take samples for TLC detection until the reaction is completed;

[0039] S3, after the reaction is completed, filter, recycle the titanium dioxide powder and platinum metal, distill to remove toluene, and dry at 95° C. to obtain crude epiandrosterone;

[0040] S4, take 95 g of the crude epiandrosterone obtained in step S3, dissolve in 3 times the mass of methanol, add 0.02 times the mass of activated carbon, reflux at 60-70°C for 2 hours, suction filter and concentrate to a paste at 50-55°C, and pump The filtered methanol is recycled, cooled and crystallized at 5°C, and the crystals are filtered and dried to obtain the fine epiandrosteron...

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Abstract

The invention provides a novel technology for synthesizing epiandrosterone by adopting 4-androstenedione through selective hydrogenation reducing.Epiandrosterone is synthesized by adopting 4-androstenedione through selective hydrogenation reducing, therefore, the reaction path is greatly shortened, generation of an intermediate reaction by-product is prevented, and the product purity and yield are high; in addition, the reaction raw material consumption is lower, the cost is reduced, and the concept requirement for green production is met.

Description

technical field [0001] The invention relates to a synthesis technology of epiandrosterone, in particular to a new process for synthesizing epiandrosterone through selective reduction and hydrogenation of 4-androstenedione. Background technique [0002] Epiandrosterone, the molecular formula is C 19 h 30 o 2 , for steroid hormone drugs. [0003] At present, the process for synthesizing epiandrosterone in industry is: (1) using diene as raw material, first preparing dehydroepiandrosterone, and then synthesizing epiandrosterone under a hydrogen reducing atmosphere; (2) using 4-androstene Using ketone as raw material, dehydrogenate is prepared first, and then epiandrosterone is synthesized under hydrogen reducing atmosphere. [0004] Above synthetic technique, reaction route is longer, and side reaction is more, causes product purity and yield rate to be lower, raw material consumption is higher, and cost is higher. Contents of the invention [0005] In view of this, the ...

Claims

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Application Information

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IPC IPC(8): C07J1/00
CPCC07J1/0011
Inventor 闻开学陈春笋
Owner 湖北省丹江口开泰激素有限责任公司
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