反应详情

A mixture of 1.76 g of the triethylamine salt of diflunisal and 1.0 g of 1-chloroethyl ethyl carbonate are heated in an oil bath at 100°-110° with magnetic stirring for 3 hours. The reaction mixture is then cooled to room temperature and 5 ml of methanol are added. After cooling to 0°-5°, the resulting precipitate is collected by filtration, washed with 3 ml of cold methanol then with 5 ml of 10% ethyl ether in hexane. After air drying there is obtained 1.38 g (75%) of 1-(ethoxycarbonyloxy)ethyl 5-(2,4-difluorophenyl)salicylate, m.p. 76°-78°.

1. temperatureare heated in an oil bath at 100°-110°
2. temperatureAfter cooling to 0°-5°
3. filtrationthe resulting precipitate is collected by filtration
4. washwashed with 3 ml of cold methanol
5. customAfter air drying there