反应详情

温度

40 °C

4-(pyrrolidino) tricyanovinylbenzene was prepared by mixing 1-phenylpyrrolidine (1.0 g, 6.8 mmol) with tetracyanoethylene (0.9 g, 7 mmol) in 10 mL dimethylformamide at 0° C. The reaction mixture was stirred at room temperature for three hours and at 40° C. for another ten hours. The reaction mixture was quenched with 25 mL water and the dark red colored aqueous solution was extracted with 150 mL methylene chloride and washed several times with water (150 mL). The organic layer was then separated, dried over Na2SO4 and evaporated. The crude products were purified through a silica gel column. The column was eluted with a 1:1 ratio solution of methylene chloride and hexane to yield 1.7 g of the pure product 4 (90% yield).

1. customThe reaction mixture was quenched with 25 mL water
2. extractionthe dark red colored aqueous solution was extracted with 150 mL methylene chloride
3. washwashed several times with water (150 mL)
4. customThe organic layer was then separated
5. dry with materialdried over Na2SO4
6. customevaporated
7. customThe crude products were purified through a silica gel column
8. washThe column was eluted with a 1:1 ratio solution of methylene chloride and hexane