HRID922130

反应详情

EQUATION

反应方程式

HRID 922130 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

20.50 g (80.32 mmol) of methyl 1-amino-4-methoxy-4-(trifluoromethyl)cyclohexanecarboxylate (Example 22A) and 8.13 g (80.32 mmol) of triethylamine were dissolved in 280 ml of dichloromethane. 21.70 g (73.02 mmol) of (4′-chloro-3′-fluoro-4-methylbiphenyl-3-yl)acetyl chloride (Example 4AA), dissolved in 280 ml of dichloromethane, were added dropwise to this solution, and the reaction mixture was stirred at room temperature overnight. For work-up, the mixture was diluted with dichloromethane and the organic phase was washed with aqueous saturated sodium bicarbonate solution and with aqueous 1% strength citric acid. After drying over sodium sulphate, the organic phase was concentrated and the product was dried. This gave 37.05 g (98% of theory) of the title compound as a beige powder.

WORKUP

后处理

  1. additionwere added dropwise to this solution
  2. washthe organic phase was washed with aqueous saturated sodium bicarbonate solution and with aqueous 1% strength citric acid
  3. dry with materialAfter drying over sodium sulphate
  4. concentrationthe organic phase was concentrated
  5. customthe product was dried