HRID270249

反应详情

EQUATION

反应方程式

HRID 270249 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1.4 l of nitrobenzene were cooled in an ice bath and treated in succession at a maximum temperature of 6° C. with 492.6 g (3.656 mol) of aluminum chloride and 700 g (3.355 mol) of 4-trifluoromethyl-2-fluoro-benzoyl chloride in 350 ml of nitrobenzene. The mixture was stirred (15 min) and 427.5 g (3.388 mol) of 3-fluoroanisole were added slowly so that the temperature did not rise above 6° C. The solution was left to warm to room temperature, stirred 2 h at this temperature, poured on to ice-water (2.5 l) and extracted with methylene chloride. The organic phase was washed with water and concentrated. After crystallization from THF (1.2l)/hexane (4.2l), 237 g (24%) of (2-Fluoro-4-methoxy-phenyl)-(4-trifluoromethyl-phenyl)-methanone were obtained, MS: 298 (M).

WORKUP

后处理

  1. additionwere added slowly so that the temperature
  2. customdid not rise above 6° C
  3. waitThe solution was left
  4. extractionextracted with methylene chloride
  5. washThe organic phase was washed with water
  6. concentrationconcentrated
  7. customAfter crystallization from THF (1.2l)/hexane (4.2l)