HRID4978

反应详情

EQUATION

反应方程式

HRID 4978 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1-Azabicyclo[2.2.2]octan-3-one (3.86 g) was heated at reflux with 2-chlorobenzaldehyde (8.33 ml), potassium hydroxide (0.4 g) and methanol (60 ml) under nitrogen for 2.5 hours. The volatiles were removed in vacuo and the residue washed with sodium hydrogen carbonate. This was extracted (×4) with dichloromethane. The organic layer was washed with water and dried (MgSO4). The dichloromethane was removed in vacuo and the residue recrystallised from methanol-dichloromethane, to afford the title compound as yellow crystals:

WORKUP

后处理

  1. customThe volatiles were removed in vacuo
  2. washthe residue washed with sodium hydrogen carbonate
  3. extractionThis was extracted (×4) with dichloromethane
  4. washThe organic layer was washed with water
  5. dry with materialdried (MgSO4)
  6. customThe dichloromethane was removed in vacuo
  7. customthe residue recrystallised from methanol-dichloromethane