HRID1961456

反应详情

EQUATION

反应方程式

HRID 1961456 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

14.24 g (107 mmol) AlCl3 was added portionwise to a solution of 6.98 g (40 mmol) 4-phenylcyclohexanone and 4.51 ml (53.3 mmol) oxalylchloride in 200 ml CH2Cl2 at 0° C. Stirred at 0° C. for 1 h and at r.t. for 2 h. Cooled to 0° C. and aqueous NH3 was added carefully until pH>10. The mixture was diluted with CH2Cl2 and water. The mixture was filtered to remove solids. The phases were separated. The organic phase was dried (MgSO4) and concentrated. Gave 4.8 g (55%) of the title compound. Used in the next step without further purification.

WORKUP

后处理

  1. temperatureCooled to 0° C.
  2. filtrationThe mixture was filtered
  3. customto remove solids
  4. customThe phases were separated
  5. dry with materialThe organic phase was dried (MgSO4)
  6. concentrationconcentrated