HRID1961456
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureCooled to 0° C.
- filtrationThe mixture was filtered
- customto remove solids
- customThe phases were separated
- dry with materialThe organic phase was dried (MgSO4)
- concentrationconcentrated