反应详情

To a solution of o-toluamide (13.5 g, 0.100 mol) in dichloromethane (150 mL) was added a solution (1.0 M, 106 mL, 0.106 mol) of triethyloxonium tetrafluoroborate in dichloromethane. The resulting mixture was stirred at room temperature for 14 h. Two-thirds of dichloromethane was evaporated under reduced pressure. After addition of ether (400 mL) to the concentrate, the mixture was stirred for 3 h under ice-cooling. Precipitates were collected by filtration, washed with ether, and dried in vacuo to give 21.7 g (86%) of ethyl 2-methylbenzimidate hydrotetrafluoroborate as a colorless solid.

1. customTwo-thirds of dichloromethane was evaporated under reduced pressure
2. additionAfter addition of ether (400 mL) to the concentrate
3. stirringthe mixture was stirred for 3 h under ice-
4. temperaturecooling
5. customPrecipitates
6. filtrationwere collected by filtration
7. washwashed with ether
8. customdried in vacuo