反应详情

The amine produced in Procedure 90, 14.5 g. (0.079 mole) was dissolved in 50 ml. of methanol and treated with a solution 9.1 g. (0.086 mole) of cyanogen bromide in 30 ml. of methanol in dropwise fashion. The warm solution was cooled to room temperature which resulted in the formation of a precipitate. The mixture was kept with stirring for 1/2 hr. and then a portion of the solvent was removed by distillation in vacuo. The solid product which separated was collected on a filter, washed with Et2O, and air dried, yield 16 g., m.p. 270°-272°.

1. dissolution(0.079 mole) was dissolved in 50 ml
2. customresulted in the formation of a precipitate
3. customand then a portion of the solvent was removed by distillation in vacuo
4. customThe solid product which separated
5. customwas collected on a filter
6. washwashed with Et2O, and air
7. customdried