HRID2043075

反应详情

EQUATION

反应方程式

HRID 2043075 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

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 (0.9 mmol) of isopropyl 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 dried over sodium sulfate and filtered after addition of activated carbon. The crude product obtained after removal of the solvent was recrystallized from methanol. 142 mg (60%) of the title compound were obtained as a colorless solid.

WORKUP

后处理

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