反应详情

温度

-15 °C

A solution of 4-[4-(1-cyclopentyl)-1-piperazinyl]benzenamine (5.7 g, 22.4 mmol) (from Step B above) in N,N-dimethylformamide (75 mL) was added dropwise over 20 min to a cooled (−15° C.) solution of thiocarbonyldiimidazole (4 g, 22.5 mmol) (Aldrich) in N,N-dimethylformamide (40 mL). After the addition was complete, the mixture was stirred at −15° C. for 20 min, then the cooling bath was removed and the solution was stirred for 1 hr. then poured into ice-water (1500 mL), stirred for 30 min. then the precipitate filtered and washed with water and dried under vacuum to give 4-cyclopentyl-1-(4-isothiocyanatophenyl)piperazine (6 g, 93%)

1. additionAfter the addition
2. customthe cooling bath was removed
3. stirringthe solution was stirred for 1 hr
4. additionthen poured into ice-water (1500 mL)
5. stirringstirred for 30 min.
6. filtrationthe precipitate filtered
7. washwashed with water
8. customdried under vacuum