Unlock instant, AI-driven research and patent intelligence for your innovation.

Technique for synthesizing the exemestane

A technology for exemestane and synthesis process, applied in the field of exemestane synthesis technology, can solve the problems of high industrialization cost and low yield, and achieve the effects of easy availability of raw materials, high yield and simple process route

Inactive Publication Date: 2007-05-23
NANJING CHANGAO PHARM CO LTD
View PDF2 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] 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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Technique for synthesizing the exemestane
  • Technique for synthesizing the exemestane
  • Technique for synthesizing the exemestane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment Construction

[0029] l, Synthesis of 6-methylene-androst-4-ene 3,17-dione

[0030] 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 for another 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)

[0031] 2. Synthesis of Exemestane

[0032] 6-methylene-androst-4-ene 3,17-dione 40g (0.13mol), toluene 1600ml, 3,5-dinitrobenzoic acid 20g, heated to reflux, added DDQ 60g (...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

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 dichlorodicyanobenzoquinone (2,3-dichloro-5,6-dicyano-1,4-benzoquinone, referred to as DDQ) The finished product is obtained, and the total yield of the two steps is 10-20% (K-Afmen et al. Tetrahedron 20:597, 1964). [0004] [0005] 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. [0006] 2. Using androst-4-ene-3,17-dione a...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): C07J1/00
Inventor 黄海燕宋祥珍顾天明
Owner NANJING CHANGAO PHARM CO LTD