反应详情

温度

60 °C

(±)-cis-2-Pyrrolidinyl-N-methylcyclohexylamine (3 gm) was combined with anhydrous dimethylformamide (70 ml) and warmed to 60° C. 2-(3,4-dichlorophenyl)ethyl methanesulfonate (14 gm) was added to the warm amine solution over 3 days. The reaction mixture was diluted to 500 ml with water and extracted with chloroform. The combined extracts were washed with water and treated with a solution of hydrogen bromide in methanol. The solution was concentrated on a rotary evaporator and the residual dimethylformamide removed by distillation under high vacuum. The residue was triturated with 2-propanol to provide a white solid. The solid was recrystallized from 2-propanol. Analytical data are reported in Table I.

1. extractionextracted with chloroform
2. washThe combined extracts were washed with water
3. additiontreated with a solution of hydrogen bromide in methanol
4. concentrationThe solution was concentrated on a rotary evaporator
5. customthe residual dimethylformamide removed by distillation under high vacuum
6. customThe residue was triturated with 2-propanol
7. customto provide a white solid
8. customThe solid was recrystallized from 2-propanol