Technique for synthesizing the exemestane

A technology of exemestane and synthesis process, which is applied in the field of synthesis process of exemestane, can solve the problems of low yield and high cost of industrialization, and achieve the effect of easy-to-obtain raw materials, high yield and simple process route

Inactive Publication Date: 2003-05-07
NANJING CHANGAO PHARM CO LTD
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  • Summary
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  • Description
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AI Technical Summary

Problems solved by technology

[0009] The technical problem to be solved by the present invention is the problem that the prior art yield is not high and the industrialization cost is high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment Construction

[0025] 1. Synthesis of 6-methylene-androst-4-ene 3,17-dione

[0026] Androstenedione 40g (0.14mol), tetrahydrofuran 260ml, absolute ethanol 40ml, triethyl orthoformate 40ml (0.24mol), p-toluenesulfonic acid 1.04g (6.04mmol), add to the reactor in turn, 40-45℃ After stirring the reaction for 1 hour, add 1.04 g of p-toluenesulfonic acid, react for 1 hour, then add 15.6 ml (0.14 mol) of N-methylaniline, 18 ml (0.22 mol) of 37% formaldehyde, and maintain this temperature for 2 hours, cool to Below 20°C, add 100ml of concentrated hydrochloric acid dropwise, after the addition, continue to react for 1 hour, cool to 0-5°C, add 700ml of water, stir and react for 1 hour, filter with suction, wash with water, and dry to obtain 28.6g of yellow solid with a yield of 68.6 %, m.p.159-162°C (literature value 160-163°C)

[0027] 2. Synthesis of Exemestane

[0028] 6-methylene-androst-4-ene 3,17-dione 40g (0.13mol), toluene 1600ml, nitrobenzoic acid 20g, heated to reflux, added DDQ 60g (0.26...

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Abstract

A process for synthesizing Yiximeitan includes such steps as synthesizing 6-methylene-androsta-4-ene 3,17-dione, synthesizing crude Yiximeitan, and refining. Its advantage is high output rate.

Description

technical field [0001] The invention relates to a synthesis process of exemestane. Background technique [0002] At present, there are three main synthetic processes of exemestane: [0003] 1. Using androst-4-ene-3,17-dione as raw material, heat and reflux for 6 hours in the presence of methylal and phosphorus oxychloride to obtain androst-6-methylene-4-ene- 3,17-diketone, the yield is 36%, and then dehydrogenated by DDQ to obtain the finished product, the total yield of the two steps is 10-20% (K.Afmen et al. Tetrahedron 20:597, 1964). [0004] The starting material of this process, androst-4-ene-3,17-dione, can be obtained from dehydroepiandrosterone through Woshi oxidation, but the total yield of this process route is low, and the industrialization cost is predicted to be high. Bad production. [0005] 2. Obtained from androst-4-ene-3,17-dione as raw material, after methylation at the 6-position, bromination and secondary debromination (...

Claims

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Application Information

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IPC IPC(8): C07J1/00
Inventor 黄海燕宋祥珍顾天明
Owner NANJING CHANGAO PHARM CO LTD
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