HRID1280775

反应详情

EQUATION

反应方程式

HRID 1280775 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

20 g (106 mmol) 4-(3-cyanoprop-1-yl)-piperidin hydrochloride, 40.2 g (127 mmol) bis(2-chlorophenyl)-bromomethane and 35.2 g (254 mmol) potassium carbonate are heated to boiling in 90 ml acetone for six hours. After cooling, the mixture is freed from solution under vacuum. The residue is dispersed between 90 ml tolueneand 90 ml water. The aqueous phase is extracted with 10 ml tolueneand the combined organic phases are washed with 10 ml water. The organic phase is concentrated and the residue is chromatographically purified over silica gel with CHCL3. Yield: 11.2 g (27%).

WORKUP

后处理

  1. temperatureAfter cooling
  2. additionThe residue is dispersed between 90 ml
  3. extractionThe aqueous phase is extracted with 10 ml tolueneand the combined organic phases
  4. washare washed with 10 ml water
  5. concentrationThe organic phase is concentrated
  6. customthe residue is chromatographically purified over silica gel with CHCL3