Purification method of small-grain size danazol

A purification method, the technology of danazol, which is applied in the field of preparation of raw materials, can solve the problems of large particle size differences and unsuitability for pharmaceutical preparations

Inactive Publication Date: 2018-09-28
WEIHAI GUANBIAO INFORMATION TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the method introduced in this patent cannot produce large differences in particle size, which is not suitable for the use of pharmaceutical preparations

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Step 1 Add 7g of crude danazol to 100ml of acetone, stir to dissolve; add 0.07g of activated carbon, stir, and filter;

[0017] In the second step, the temperature of the filtrate obtained in the first step is lowered to -10°C and maintained, and under stirring, 120 ml of an aqueous ethanol solution is added to the first step as a solvent; in the aqueous ethanol solution, the volume ratio of ethanol to water is 1:0.7; The ethanol aqueous solution was controlled to be added within 1 hour; after crystals were precipitated, the stirring was continued for 2.5 hours; the stirring speed was 100 revolutions per minute.

[0018] The third step is to filter, and the filter cake is washed with the ethanol aqueous solution described in the second step. Dry at 80°C. The refined product of Dedanazol has a purity of 99.64% by HPLC, a yield of 90.12%, a melting point of 223.2°C, and a D90 of 30 microns.

Embodiment 2

[0020] Step 1: Add 16g of crude danazol into acetone, stir to dissolve; add 0.48g of activated carbon, stir, and filter;

[0021] In the second step, the filtrate obtained in the first step is cooled to 0° C. and maintained, and under stirring, 300 ml of ethanol aqueous solution is added to the first step solvent amount; in the ethanol aqueous solution, the volume ratio of ethanol to water is 1:1.4; ethanol The aqueous solution was controlled to be added within 1 hour; after crystals were precipitated, the stirring was continued for 5 hours; the stirring speed was 160 revolutions per minute.

[0022] The third step is to filter, and the filter cake is washed with the ethanol aqueous solution described in the second step. Dry at 80°C. The refined product of Dedanazol, the purity by HPLC is 99.82%, the yield is 91.08%, and the temperature is 223.6°C. D90 is 16 microns.

Embodiment 3

[0024] Add 12g of crude danazol into acetone, stir to dissolve; add 0.24g of activated carbon, stir, and filter;

[0025] In the second step, the filtrate obtained in the first step is cooled to -5°C and maintained, and under stirring, 200ml of ethanol aqueous solution is added to the first step solvent amount; in the ethanol aqueous solution, the volume ratio of ethanol to water is 1:1.1, The aqueous ethanol solution was controlled to be added within 1 hour; after crystals were precipitated, the stirring was continued for 4 hours; the stirring speed was 180 revolutions per minute.

[0026] The third step is to filter, and the filter cake is washed with the ethanol aqueous solution described in the second step. Dry at 80°C. The refined product of Dedanazol, the purity by HPLC method is 99.78%, the yield is 91.67%, 223.5℃. D90 is 10 microns.

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Abstract

The invention relates to a purification method of small-grain size danazol, and belongs to the technical field of crude drug preparation. According to the technical scheme, firstly, crude danazol is added into acetone, and stirring is conducted for dissolution; activated carbon which is 1-3% of the crude danazol is added, and stirring and filtering are conducted; filter liquor is cooled to -10-0 DEG C, the temperature is maintained, and ethanol water which is 1.2-3 times of the solvent in the step 1 is added in a fed-batch manner; stirring is conducted for crystallization; filtering is conducted, and a filter cake is washed with the ethanol water in the step 2; drying is conducted at 80 DEG C. By means of the method, a high-purity danazol crude drug with a small grain size is obtained.

Description

technical field [0001] The invention relates to a method for purifying danazol, which belongs to the technical field of raw material medicine preparation. Background technique [0002] Danazol, also known as Danazol, Anconazole, Ethyl Testosterol, Ethyl Androstenazole, chemical name 17α-pregna-2,4-diene-20-alkyno[2,3-d]isox Azol-17β alcohol has weak androgenic activity, and has protein assimilation and anti-estrogen effects. It belongs to gonadotropin inhibitors and is used clinically to treat endometriosis, fibrocystic breast disease, and hereditary vascular disease. Edema, gynecomastia, precocious puberty, thrombocytopenic purpura, hemophilia and lupus erythematosus, etc. [0003] Danazol is a steroidal heterocyclic compound, a derivative of the androgen 17α-ethynyl testosterone. Danazol is insoluble in water. In order to improve the dissolution rate of the preparation, measures to control the particle size of the raw material drug are generally taken. US patents 200200...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J71/00
CPCC07J71/0063
Inventor 孙爱梅
Owner WEIHAI GUANBIAO INFORMATION TECH
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