反应详情

温度

6 °C

9.7 g (61.2 mmol) of N-methyl-N′-(3-hydroxypropyl)piperazine dissolved in 10 ml of acetonitrile are added dropwise to a solution of 100 ml of acetonitrile and 40 ml of 4 N HCl in dioxane and cooled using a water bath that the internal temperature did not exceed 40° C. 8 ml (66.3 mmol) of trichloromethyl chloroformate in 10 ml of acetonitrile are subsequently added dropwise with ice-cooling at an internal temperature of 2-10° C., and the mixture is subsequently stirred at room temperature for 15 h. The precipitate formed is filtered off with suction, washed with acetonitrile, and the residue is dried in vacuo.

1. temperaturecooled
2. customdid not exceed 40° C
3. customThe precipitate formed
4. filtrationis filtered off with suction
5. washwashed with acetonitrile
6. customthe residue is dried in vacuo