反应详情

温度

20 °C

Methanethiol (278 g, 5.78M) was added during 20 minutes to a stirred mixture of acetone (5 litres) and potassium carbonate (593 g, 4.29M) at −15° C. A solution of 2-nitro-4-trifluoromethylbenzonitrile (618 g, 2.86M) in acetone (500 ml) was added during 10 minutes. The mixture was allowed to warm to 20° C. with stirring for 23 hours and then heated at 55° C. for 2 hours to remove most of the methanethiol and then flushed with nitrogen for 4 hours. The mixture was poured onto ice/water, the solid filtered off, washed and dried to give 2-methylthio-4-trifluoromethylbenzonitrile (550 g). The yield of product was 89%.

1. temperatureheated at 55° C. for 2 hours
2. customto remove most of the methanethiol
3. customflushed with nitrogen for 4 hours
4. additionThe mixture was poured onto ice/water
5. filtrationthe solid filtered off
6. washwashed
7. customdried