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A kind of preparation method of dehydromethyl testosterone

A technology of hydromethyl testis and bromine, applied in the directions of steroids, organic chemistry, etc., can solve the problems of complicated process operation, long synthesis route and high production cost, and achieves wide source of raw materials, short synthesis route and reduced production cost. Effect

Active Publication Date: 2019-11-05
HUNAN KEREY BIOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to provide a new preparation method of dehydromethyltestosterone, which overcomes many shortcomings in the traditional production process, such as expensive synthetic raw materials, long synthetic route, complicated process operation, difficult environmental protection treatment, high production cost, etc.

Method used

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  • A kind of preparation method of dehydromethyl testosterone
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Examples

Experimental program
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Effect test

Embodiment 1

[0019] A, the preparation of double bromide

[0020] In a 2000ml three-neck bottle, add 100g of metandrolone, 200ml of dioxane, 80g of 25% hydrobromic acid in acetic acid solution, stir to make the system strongly acidic, control the temperature at 25-30 degrees, and slowly add 80g of bromine The solution made of dioxane and 600ml dioxane should be dripped within about 1.0-1.5 hours. After the dripping, continue to keep warm at 25-30 degrees for 4-6 hours. TLC confirms the reaction end point. After the reaction, slowly Add 200ml of 30% sodium hydrosulfite solution dropwise to completely destroy bromine, then concentrate under reduced pressure to recover 90-95% of dioxane, after concentration, cool down to 10-15 degrees, add 600ml of tap water, stir and crystallize for 3 -4 hours, centrifuged, washed with water until neutral, dried under vacuum below 40°C to obtain 146.8g of the bisbromide 2,4-dibromo-menandrolone, with HLPC content of 98.5%, moisture content of 3.5%, and weigh...

Embodiment 2

[0024] A, the preparation of double bromide

[0025] In a 2000ml three-necked flask, add 100g of methandrolone, 500ml of toluene, and 80g of 25% hydrobromic acid aqueous solution, stir to make the system strongly acidic, control the temperature at 25-30 degrees, and slowly add 80g of bromine and 300ml of DMF dropwise The prepared solution should be dropped within about 1.0-1.5 hours. After the drop, continue to keep warm at 25-30 degrees for 4-6 hours. TLC confirms the reaction end point. After the reaction, slowly add 200ml of 30% insurance powder aqueous solution to completely destroy bromine, then wash twice with 600 ml of tap water, separate the water, dry with 50 g of anhydrous magnesium sulfate, and concentrate under reduced pressure to recover 90-95% of the mixed solvent of toluene and DMF. After concentration, Cool down to 10-15 degrees, add 600ml of tap water, stir and crystallize for 3-4 hours, centrifuge, wash with water until neutral, and dry in vacuum below 40 deg...

Embodiment 3

[0029] A, the preparation of double bromide

[0030]In a 2000ml three-necked bottle, add 100g of methandrolone, 500ml of chloroform, and 80g of 25% hydrobromic acid in glacial acetic acid, stir to make the system strongly acidic, control the temperature at 25-30 degrees, and slowly add 80g of bromine and The solution made of 300ml chloroform should be dripped within about 1.0-1.5 hours. After the dripping, continue to keep warm at 25-30 degrees for 4-6 hours. TLC confirms the reaction end point. After the reaction, slowly add 200ml 30% Sodium hydrosulfite aqueous solution to completely destroy bromine, then wash twice with 600 ml tap water, separate water, dry with 50 g of anhydrous magnesium sulfate, and concentrate under reduced pressure to recover 90-95% of chloroform solvent. After concentration, cool down to 10-15 degrees, add 600ml of tap water, stir and crystallize for 3-4 hours, centrifuge, wash with water until neutral, and vacuum dry below 40 degrees to obtain 147.6g...

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Abstract

The invention discloses a method for preparing metandienone. The method comprises the following steps: dissolving mestanolone into an organic solvent, performing a reaction with bromine for 4-6 hours in a strong acid solution, and performing bibromination at a 2,4 site of mestanolone molecules so as to obtain 2,4-bibromine mestanolone; further dissolving the 2,4-bibromine mestanolone into an organic solvent, performing a reaction for bidebromination with a debromination agent for 2-6 hours, and implementing two steps of reactions to synthesize a crude product of metandienone; decoloring the crude product with activated carbon in low-carbon alcohol less than C4, and performing recrystallization, thereby obtaining a methyltestosterone product, wherein the content of HPLC is 99.0-99.5%, the melting point is 162-167 DEG C, and the total yield of a synthesis weight is 75-78%. The method disclosed by the invention has the advantages of being wide in raw material source, short in synthesis route, simple, convenient and environmentally friendly in process, high in product yield, good in quality, and the like, the production cost of the method is reduced by 30-35% when being compared with that of a conventional method, the solvent can be recycled and repeatedly used, and thus the method is both economic and environmental-friendly and is very beneficial to industrial production.

Description

technical field [0001] The invention belongs to the preparation technology of steroid hormone medicine, and in particular relates to a preparation method of anabolic hormone medicine dehydromethyltestosterone. Background technique [0002] Dehydromethyltestosterone, commonly known as Dianabol, chemically named 17a-methyl-androst-1,4-dien-3-one-17-ol, is an anabolic hormone drug with androgenic effects, Clinically, it is mainly used for the treatment of burns, trauma and postoperative treatment, and the treatment of malnutrition in children. It is also used for the treatment of aplastic anemia, the recovery period of chronic wasting diseases, and patients who have been treated with adrenal corticosteroids for a long time or in large quantities. The market is huge. . The traditional production method of demethyl testosterone is to extract diosgenin from yam plant, after protection, oxidative cracking, and elimination, the key intermediate acetic acid gestational dienolone (re...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J1/00
CPCC07J1/0037
Inventor 胡爱国甘红星谢来宾吴来喜
Owner HUNAN KEREY BIOTECH
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