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A kind of preparation method of dehydromethyl testosterone product

A technology of hydromethyl testosterone and products, applied in the field of preparation of anabolic hormone drug dehydromethyl testosterone products, can solve the production cost of dehydromethyl testosterone and the increase in market price, saponin, diene production cost problems such as growth, rising planting costs, etc., to achieve the effect of reducing the cost of production raw materials, high product yield, and reduced production costs

Active Publication Date: 2020-11-06
HUNAN KEREY BIOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the extraction of diosgenin, oxidative cracking, Beckmann rearrangement, acid and alkali hydrolysis, DDQ dehydrogenation and other processes produce more waste water, which is difficult to treat and easy to pollute the environment; the Oxide oxidation process used in production requires water Steam distillation, high water consumption and energy consumption
More importantly, with the depletion of wild yam plant resources, and the artificial planting of yam plants, the production costs of saponin and dienes have doubled due to the increasing cost of artificial and chemical fertilizers, resulting in dehydromethylation. Significant increase in production cost and market price of testosterone has had a major impact on the global dehydromethyltestosterone drug market

Method used

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  • A kind of preparation method of dehydromethyl testosterone product
  • A kind of preparation method of dehydromethyl testosterone product

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Experimental program
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Effect test

Embodiment 1

[0037] A. Preparation of Grignard reagents

[0038]In a 1000ml three-neck flask, add 35g of magnesium powder and 800ml of tetrahydrofuran, stir, keep warm at 30-35°C, and feed 98g of methyl chloride. After the passage, continue to stir and react for 4 to 6 hours until the magnesium powder basically disappears, and the Grignard Reagent spare;

[0039] B, the preparation of dehydromethyltestosterone

[0040] In a 1000ml three-neck flask, add 100g IDD and 500ml THF, stir and heat up to 50-55°C, slowly add about 800ml of the Grignard reagent solution prepared above, dropwise for about 1-1.5 hours, then continue to keep warm and stir for 2~ After 3 hours, TLC detects the end point of the reaction. After the reaction, slowly add 2N hydrochloric acid to pH 2-3. After the drop, continue the hydrolysis reaction at 50-55°C for 2-3 hours. TLC detects that the hydrolysis is complete. After the reaction, reduce the pressure About 90-95% THF was concentrated, and the recovered THF was use...

Embodiment 2

[0044] A. Preparation of Grignard reagents

[0045] In a 1000ml three-necked flask, add 35g of magnesium powder and 800ml of tetrahydrofuran, stir, keep warm at 40-45°C, and feed 120g of methyl bromide. After the passage, continue to stir and react for 2 to 3 hours until the magnesium powder basically disappears to obtain the Grignard reagent spare;

[0046] B, the preparation of dehydromethyltestosterone

[0047] In a 1000ml three-neck flask, add 100g IDD and 500ml toluene, stir and heat up to 50-55°C, slowly add about 800ml of the Grignard reagent solution prepared above, dropwise for about 1-1.5 hours, then continue to keep warm and stir for reaction 2 ~3 hours, TLC detects the end point of the reaction. After the reaction, slowly add 2N hydrochloric acid to PH2-3. After the drop, continue the hydrolysis reaction at 50-55°C for 2-3 hours. The mixture of THF and toluene about 90-95% was concentrated under reduced pressure, and the recovered mixture of THF and toluene was u...

Embodiment 3

[0051] A. Preparation of Grignard reagents

[0052] In a 1000ml three-necked flask, add 35g of magnesium powder and 800ml of ether, stir, keep warm at 30-35°C and add 150g of methyl iodide dropwise. After passing through, continue to stir and react for 4 to 6 hours until the magnesium powder basically disappears to obtain Grignard Reagent spare;

[0053] B, the preparation of dehydromethyltestosterone

[0054] In a 1000ml three-neck flask, add 100g IDD and 500ml benzene, stir and heat up to 50-55°C, slowly add about 800ml of the Grignard reagent solution prepared above, dropwise for about 1-1.5 hours, then continue to keep warm and stir for reaction 2 ~3 hours, TLC detects the end point of the reaction. After the reaction, slowly add 2N hydrochloric acid to pH2-3. After the drop, continue the hydrolysis reaction at 50-55°C for 2-3 hours. Concentrate under high pressure to get about 90-95% of the mixture of ether and benzene, and the recovered mixture of ether and benzene can...

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Abstract

The invention provides a preparation method of a metandienone product. The preparation method comprises the following steps that 1,4-androstenedione, namely IDD, is adopted as a raw material, in the presence of methylmagnesium chloride, an organic solvent and acid, alpha-CH3 and beta-OH are introduced at the 17 position, and metandienone is prepared; and then the obtained metandienone is heated byactivated carbon in acetone or lower alcohol below C4 for reflow discoloration and is recrystallized, and the metandienone product is obtained. According to the preparation method, the IDD serves asthe raw material to prepare the metandienone, compared with a traditional method adopting diosgenin as a raw material, the raw material source is wide, a process is economic and environmentally friendly, and the production cost is significantly lowered. Compared with a traditional production method, according to the preparation method, a synthesis route is short, the process is easy, convenient and environmentally friendly, the product yield is high, the quality is good, and the production raw material cost is lowered by 40-45% by calculating through the current raw material price.

Description

technical field [0001] The invention belongs to the preparation technology of steroid hormone medicine, and in particular relates to a preparation method of an anabolic hormone medicine dehydromethyltestosterone product. Background technique [0002] Dehydromethyltestosterone is an anabolic hormone drug, which has the effect of androgen. It is mainly used clinically for burns, trauma and postoperative treatment, and for the treatment of malnutrition in children. It is also used for the treatment of aplastic anemia, chronic There is a large market for patients in the recovery period of wasting diseases and patients who have been using adrenal corticosteroids for a long time or in large quantities. [0003] The traditional production method of dehydromethyltestosterone is to extract diosgenin from the yam plant, and through protection, oxidation, cracking, and elimination, the key intermediate acetic acid gestational dienolone (diene for short) obtained is used as a raw materi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J1/00
CPCC07J1/0037
Inventor 甘红星吴来喜胡爱国
Owner HUNAN KEREY BIOTECH
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