HRID47530

反应详情

EQUATION

反应方程式

HRID 47530 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1-[1-(Piperidin-4-yl)piperidin-4-yl]-1,3-dihydro-2H-benzimidazol-2-one-dihydrochloride (37.3 mg) was dissolved in 3 ml of chloroform, and to which 21 μl of ethyl chloroformate and 84 μl of triethylamine were successively added under cooling with ice, followed by overnight stirring at room temperature. To the reaction liquid saturated aqueous sodium hydrogencarbonate solution was added and extracted with chloroform. The organic layer was washed with saturated. brine, dried over anhydrous sodium sulfate and then the solvent was distilled off. The resulting residue was purified by silica gel column chromatography (chloroform/methanol=10/1) to provide 41.7 mg of the title compound as a colorless oil.

WORKUP

后处理

  1. temperatureunder cooling with ice
  2. additionwas added
  3. extractionextracted with chloroform
  4. washThe organic layer was washed with saturated
  5. dry with materialbrine, dried over anhydrous sodium sulfate
  6. distillationthe solvent was distilled off
  7. customThe resulting residue was purified by silica gel column chromatography (chloroform/methanol=10/1)