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Dehalogenation method of 9-halogenated steroid compound and application

A steroid compound and compound technology, applied in the direction of steroid compound, organic chemistry, drug combination, etc., can solve the problems of affecting the normal production of products, high environmental protection cost, restricting normal application, etc. The effect of production applicability and high safety factor

Pending Publication Date: 2021-12-31
TIANJIN PHARMA GROUP CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Most of the above-mentioned processes use heavy metal raw materials, highly toxic raw materials, etc., causing serious pollution to the environment, high cost of environmental protection treatment or use of restricted raw materials; thus limiting the normal application of this type of reaction, and affecting the normal production of this type of product

Method used

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  • Dehalogenation method of 9-halogenated steroid compound and application
  • Dehalogenation method of 9-halogenated steroid compound and application
  • Dehalogenation method of 9-halogenated steroid compound and application

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Experimental program
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Effect test

Embodiment 1

[0061]

Embodiment 1-1

[0063] Put 10g of compound I-1, 3.4g of potassium thioacetate and 50mL of ethanol into the reaction flask at room temperature, raise the temperature to 70°C for reaction, and no compound I-1 was detected by TLC. After the reaction, concentrate the reaction solution, add water, continue Concentrate until no solvent is evaporated, dilute the concentrate in 10 times water, stir for 30 min, filter with suction, discharge, and dry to obtain Compound II-17.7g with a yield of 95.7% and an HPLC purity of 98.2%.

Embodiment 1-2

[0065] Put 10g of compound I-1, 3.9g of sodium thioacetate and 60mL of N,N-dimethylformamide into the reaction flask at room temperature, raise the temperature to 80°C for reaction, and monitor no compound I-1 by TLC. After the reaction is completed, Diluted in 30 times of water, stirred for 30 min, suction filtered, discharged, and dried to obtain Compound II-17.6g with a yield of 95.5% and a purity of 98.0%.

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Abstract

The invention provides a dehalogenation method of a 9-halogenated steroid compound and application, and relates to the technical field of chemical synthesis. The dehalogenation method of the 9-halogenated steroid compound comprises the step of reacting a compound I with sulfo fatty acid salt to obtain a 9-bit dehalogenation product compound II of the 9-halogenated steroid compound. According to the dehalogenation method of the 9-halogenated steroid compound, the compound I and the sulfo fatty acid salt react to obtain the 9-bit dehalogenation product compound II of the 9-halogenated steroid compound, reagents such as zinc powder, chromium particles or tri-n-butyltin which are high in toxicity and cause serious pollution to the environment are not used in the reaction, the dehalogenation method is green and environmentally friendly, the synthesis process is simple and easy to implement, and the production applicability is improved.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a dehalogenation method and application of a 9-halogenated steroid compound. Background technique [0002] Steroid hormone drugs (steroid hormone drugs) refer to hormone drugs containing steroidal structure in their molecular structure, which are widely used clinically and mainly include adrenocortical hormones and sex hormones. Among them, adrenal cortex hormone has various pharmacological effects such as anti-inflammation, anti-allergy, immune suppression, enhancement of stress response, anti-endotoxin and anti-shock. [0003] In the synthesis process of many corticosteroid drugs, it is necessary to perform reductive dehalogenation reaction on the 9-position halogen. Commonly used reducing agents in industry include zinc powder, chromium particles or tri-n-butyltin, etc. [0004] Zinc powder is the most used at present. [0005] J.Chem.Soc.PerkinTrans.1,1986:1621 ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J7/00A61P29/00A61P37/08A61P37/02
CPCC07J7/008C07J7/0045C07J71/0031C07J71/001A61P29/00A61P37/08A61P37/02
Inventor 任楠韩昆颖
Owner TIANJIN PHARMA GROUP CORP