反应详情

188 mg (0.5 mmol) of 4-(2-(5-chloro-2-methoxybenzamido)ethyl)piperidine-1-sulfonamide and 326 mg (1 mmol) of cesium carbonate were heated in 5 ml of N-methyl-2-pyrrolidone with 0.1 ml (1.1 mmol) of ethyl isothiocyanate at 80° C. for 10 minutes. The reaction mixture was poured onto ice/2 M hydrochloric acid and extracted three times with 10 ml of dichloromethane each time. The combined organic phases were washed with water until neutral, dried over sodium sulfate and filtered after addition of activated carbon. The crude product obtained after removal of the solvent was recrystallized from methanol/water. 80 mg (35%) of the title compound were obtained as a colorless solid.

1. additionThe reaction mixture was poured onto ice/2 M hydrochloric acid
2. extractionextracted three times with 10 ml of dichloromethane each time
3. washThe combined organic phases were washed with water until neutral,
4. dry with materialdried over sodium sulfate
5. filtrationfiltered
6. additionafter addition of activated carbon
7. customThe crude product obtained
8. customafter removal of the solvent
9. customwas recrystallized from methanol/water