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High-yield synthesis method of trenbolone acetate

A technology for the synthesis of trenbolone acetate and its synthesis method, which is applied in the field of synthesis of trenbolone acetate, and can solve the problems of low yield, many by-products, and low quality

Inactive Publication Date: 2013-02-13
YICHENG GOTO PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This route has many by-products, low quality and low yield

Method used

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  • High-yield synthesis method of trenbolone acetate

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Embodiment 1

[0021] 1. Etherification reaction: Put 80kg of alcohol into a 500L reaction tank and cool down to 0°C, start stirring, add 10kg of acetyl chloride dropwise, and control the temperature at 0-10°C. After the dropwise addition, 10 kg of estro-4,9-diene-3,17-dione was added, and stirred and kept at 10-13° C. for 2 hours. After the heat preservation is completed, the feed liquid is pumped into the sodium carbonate aqueous solution, and the temperature is controlled at 20-25°C. After the dropwise addition, the temperature is controlled at 20-25°C, stirred for 30 minutes, filtered with suction, washed with a large amount of water until neutral, and centrifuged to obtain a wet feed.

[0022] 2. Reductive hydrolysis dehydrogenation reaction: pump 100kg of methanol into a 500L reaction tank, put in the wet material of the previous step, cool down to 0°C, add 5kg of potassium borohydride, control the temperature at 0-5°C when adding, and stir after the addition is complete Keep warm for ...

Embodiment 2

[0026] Embodiment 2: The raw materials involved in the etherification reaction and the consumption were changed to 75 kg of methanol, 5 kg of acetyl chloride, and 5 kg of estro-4,9-diene-3,17-dione;

[0027] The raw materials and dosage involved in the reduction reaction are changed to 95 kg of methanol, 95 kg of wet reaction material, 4 kg of potassium borohydride, and 180 kg of dichloromethane;

[0028] The raw materials and dosage involved in the hydrolysis reaction are changed to 180kg of oil, 65kg of methanol, 18kg of dichloromethane, and 6kg of anhydrous magnesium sulfate;

[0029] The raw materials involved in the dehydrogenation reaction and the consumption are changed to 180kg of dichloromethane, 180kg of filter cake, and 6kg of DDQ;

[0030] The raw materials involved in the acylation reaction and the amount used were changed to 95 kg of benzene, 6 kg of pyridine, 6 kg of trenbolone, 0.3 kg of 4-DMAP, 6 kg of acetyl chloride, 6 kg of ethyl acetate, and 20 kg of petro...

Embodiment 3

[0032] Example 3: The raw materials and dosage involved in the etherification reaction were changed to 85 kg of methanol, 15 kg of acetyl chloride, and 15 kg of estro-4,9-diene-3,17-dione;

[0033] The raw materials and dosage involved in the reduction reaction are changed to 105kg of methanol: 105kg of wet reaction material, 10kg of potassium borohydride, and 210kg of dichloromethane;

[0034] The raw materials involved in the hydrolysis reaction and the consumption are changed to 210kg of oil, methanol, 75kg, 210kg of dichloromethane, and 15kg of anhydrous magnesium sulfate;

[0035] The raw materials involved in the dehydrogenation reaction and the consumption are changed to 210kg of dichloromethane, 210kg of filter cake, and 12kg of DDQ;

[0036] The raw materials involved in the described acylation reaction and the consumption are changed to 105 kg of benzene, 12 kg of pyridine, 12 kg of trenbolone, 0.6 kg of 4-DMAP, 12 kg of acetyl chloride, 12 kg of heptanoyl chloride, ...

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Abstract

The invention relates to a synthesis method of trenbolone acetate, which comprises the following steps: 1. etherification reaction: adding methanol, acetyl chloride and oestrogenic steroid-4,9-diene-3,17-dione into a reaction tank, stirring, regulating the pH value, carrying out vacuum filtration, washing with water, and centrifuging; 2. reduction reaction: adding potassium borohydride, stirring, regulating the pH value, washing with water, and concentrating; 3. hydrolysis reaction: adding methanol and hydrochloric acid, dotting the plate, regulating the pH value, concentrating, adding dichloromethane to be dissolved, washing with water, and dehydrating; 4. dehydrogenation reaction: rinsing with dichloromethane, adding DDQ (2,3-dichloro-5,6-dicyano-1,4-benzoquinone), dotting the plate, carrying out vacuum filtration, washing with water, concentrating, cooling, and drying to obtain trenbolone; and 5. acylation reaction: sucking in benzene and pyridine, adding the trenbolone and 4-DMAP (4-dimethylaminopyridine), dropwisely adding acetyl chloride, keeping the temperature, dotting the plate, washing with water, and concentrating. The method provided by the invention enhances the yield of the trenbolone acetate from 88-90% to 92-93.5%, and can lower the cost by 200 yuan or so per kilogram.

Description

technical field [0001] The invention relates to a synthesis method of trenbolone acetate, in particular to a synthesis method of high-yield trenbolone acetate. Background technique [0002] Trenbolone acetate is an anabolic hormone, and because of its preventive effect on mad cow disease, the demand for trenbolone acetate continues to increase. However, the synthesis route of trenbolone acetate is relatively long, and some reaction yields are extremely low, which makes it very difficult to obtain the crystallization of the final product. The traditional production process of trenbolone acetate uses 4.9(11)-diene androster 3-17-dione as the raw material, uses p-toluenesulfonic acid as the catalyst, and protects the 3-position carbonyl group. 1. Hydrolysis to obtain trenbolone; finally trenbolone and acetic anhydride undergo esterification reaction to obtain trenbolone acetate. This route has many by-products, low quality and low yield. "Fudan Journal: Medical Edition", Vol...

Claims

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Application Information

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IPC IPC(8): C07J1/00
Inventor 王延贞薛文武刘卫东张国俊
Owner YICHENG GOTO PHARMA
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