Method for converting and purifying 4-androstenedione from mother solutions of allyl ester substances and ketal substances

A technology of androstenedione and ketal, which is applied in the field of purification and preparation of 4-androstenedione, can solve the problems of low product purity and yield, high raw material consumption, long reaction route, etc., and achieve product purity and High yield, low dosage, and the effect of preventing intermediate side reaction products

Inactive Publication Date: 2016-08-31
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

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Problems solved by technology

[0005] The above synthesis process has a longer reaction route and more side reactions, res

Method used

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  • Method for converting and purifying 4-androstenedione from mother solutions of allyl ester substances and ketal substances

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] S1, 10g of the enester mother liquor obtained in the preparation process of dehydroepiandrosterone, and 10g of the ketal mother liquor obtained in the preparation process of dehydroepiandrosterone are heated and dissolved in 150g methanol, and the concentration of 10g is added to 10mol / L hydrochloric acid, react at 45°C for 2.5h, take a sample for TLC detection until the reaction is complete;

[0026] S2, adjusting the pH of the solution to 6 with an aqueous solution of sodium carbonate, adding 10 times the volume of water to precipitate crystals, centrifuging, washing with water, pulverizing, and drying to obtain crude 4-androstenedione;

[0027] Step S3: Mix 50 g of the crude 4-androstenedione obtained in step S2 with 500 g of methanol, add 2.5 g of activated carbon, reflux at 70-90° C. for 1 hour, and concentrate the crystals by suction filtration to obtain fine 4-androstenedione.

[0028] Under the detection of HPLC, the mass percent content of 4-androstenedione in ...

Embodiment 2

[0031] S1, 10g of the enester mother liquor obtained in the preparation process of dehydroepiandrosterone, and 30g of the ketal mother liquor obtained in the preparation process of dehydroepiandrosterone are heated and dissolved in 150g methanol, and 20g of concentration is added 10mol / L hydrochloric acid, react at 50°C for 3.5h, take a sample for TLC detection until the reaction is complete;

[0032] S2, adjusting the pH of the solution to 7 with an aqueous solution of sodium bicarbonate, adding 10 times the volume of water to precipitate crystals, centrifuging, washing with water, pulverizing, and drying to obtain crude 4-androstenedione;

[0033] Step S3, mixing 50 g of the crude product of 4-androstenedione obtained in step S2 with 500 g of ethyl acetate, adding 5 g of activated carbon, refluxing at 70-90° C. for 0.5 h, suctioning and concentrating the crystals to obtain the refined product of 4-androstenedione .

[0034] Under the detection of HPLC, the mass percent cont...

Embodiment 3

[0037] S1, 10g of enester mother liquor obtained in the preparation process of dehydroepiandrosterone, and 50g of ketal mother liquor obtained in the preparation process of dehydroepiandrosterone are heated and dissolved in 200g methanol, and 20g concentration is added 10mol / L hydrochloric acid, react at 55°C for 4.5h, take a sample for TLC detection until the reaction is complete;

[0038] S2, adjust the pH of the solution to 7 with aqueous sodium hydroxide solution, add 10 times the volume of water to precipitate crystals, centrifuge, wash with water, pulverize, and dry to obtain crude 4-androstenedione;

[0039] Step S3: Mix 50 g of the crude 4-androstenedione obtained in step S2 with 500 g of ethanol, add 25 g of activated carbon, reflux at 70-90° C. for 1.5 h, and concentrate the crystals by suction filtration to obtain fine 4-androstenedione.

[0040] Under the detection of HPLC, the mass percent content of 4-androstenedione in the obtained 4-androstenedione refined prod...

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Abstract

The invention discloses a method for converting and purifying 4-androstenedione from mother solutions of allyl ester substances and ketal substances. According to the method, 4-androstenedione is prepared from an allyl ester mother solution and a ketal substance mother solution which are prepared during the preparation of dehydroepiandrosterone, so that the repeated use of waste is realized, and the method is environmentally friendly and economic; the reaction route is greatly shortened, so that the generation of intermediate side reaction products is prevented, and the product purify and yield are high; and furthermore, the consumption of the reaction raw materials is relatively low, so that the cost is saved, and the requirement of green production idea is met.

Description

technical field [0001] The invention relates to the purification and preparation technology of 4-androstenedione, in particular to a method for converting and purifying 4-androstenedione from the mother liquor of enester and ketal. Background technique [0002] Epiandrosterone, the molecular formula is C 19 h 30 o 2 , for steroid hormone drugs. [0003] At present, in the preparation process of dehydroepiandrosterone, the obtained intermediate product enester and ketal mother liquor cannot be effectively utilized, resulting in waste of raw materials. [0004] In addition, the process of synthesizing epiandrosterone in industry is as follows: (1) using diene as raw material, first preparing dehydroepiandrosterone, and then synthesizing epiandrosterone under 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. [0005] Above synthetic ...

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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