反应详情

To a solution of chloroacetonitrile (3.9 ml) in methanol (166 ml) was added sodium methoxide (3.29 g), and the mixture was stirred at room temperature for 40 min under a nitrogen atmosphere. Methanesulfonic acid (7.91 ml) and 3-amino4-(cyclohexylcarbamoylmethylamino)benzonitrile (8.3 g) were added, and the mixture was stirred for 3 hours. After completion of the reaction, water (166 ml) was added and the precipitated solid was collected by filtration, and washed with a small amount of water. The obtained solid was stirred in a mixture of hexane and tetrahydrofuran, collected by filtration and dried under reduced pressure to give the title compound (9.30 g).

1. stirringthe mixture was stirred for 3 hours
2. additionwas added
3. filtrationthe precipitated solid was collected by filtration
4. washwashed with a small amount of water
5. stirringThe obtained solid was stirred in a mixture of hexane and tetrahydrofuran
6. filtrationcollected by filtration
7. customdried under reduced pressure