反应详情

温度

35 °C

2-chloro-6-fluorobenzonitrile (42.3 g, 0.27 mol) is dissolved in anhydrous diethyl ether (170 ml) and methyl magnesium bromide (291 ml of a 2.8 M solution, 0.82 mol) is added. The whole is warmed to reflux (35° C.) overnight (16 hrs.). Then the reaction mixture is quenched in ice-water (380 ml) followed by the addition of concentrated H2SO4 (95 ml). The resultant mixture is heated to 100° C. for 3 hours and stirred overnight at room temperature. Pure product is then extracted from the mixture using chloroform (45.0 g, 95.9%).

1. temperatureThe whole is warmed
2. customThen the reaction mixture is quenched in ice-water (380 ml)
3. additionfollowed by the addition of concentrated H2SO4 (95 ml)
4. temperatureThe resultant mixture is heated to 100° C. for 3 hours
5. extractionPure product is then extracted from the mixture