反应详情

温度

-15 °C

A solution of 4-[4-(cyclopropylmethyl)-1-piperazinyl]benzenamine (3.7 g, 16 mmol) (from Step B above) in N,N-dimethylformamide (50 mL) was added dropwise over 20 min to a cooled (−15° C.) solution of thiocarbonyldiimidazole (2.87 g, 16.1 mmol) (Aldrich) in N,N-dimethylformamide (25 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 h. Ice-water (1000 mL) was added and the mixture was stirred for 30 min. The solid was filtered off and washed with water and dried under vacuum. (4 g, 91%).

1. additionAfter the addition
2. customthe cooling bath was removed
3. stirringthe solution was stirred for 1 h
4. additionIce-water (1000 mL) was added
5. stirringthe mixture was stirred for 30 min
6. filtrationThe solid was filtered off
7. washwashed with water
8. customdried under vacuum