HRID568621

反应详情

EQUATION

反应方程式

HRID 568621 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 24.6 g of 2,6-difluoro benzoylchloride in 100 ml of 1,2-dichloroethane, 18.5 g of AlCl3 is added in portions over a 30 minute period. A solution of 22.5 g of 2,3-dichloroanisole in 100 ml of 1,2-dichloroethane is added thereto. The mixture is stirred for one hour and poured over 100 ml concentrated HCl and ice. The organic layer is separated and the aqueous layer extracted with CHCl3. The organic extract is washed with water, dried (Na2SO4) and evaporated to give an oil which crystallizes from hexane to yield solid 2,3-dichloro-4-methoxy-2',6'-difluorobenzophenone which upon recrystallization from ether has an mp 94°-96° C.

WORKUP

后处理

  1. customThe organic layer is separated
  2. extractionthe aqueous layer extracted with CHCl3
  3. extractionThe organic extract
  4. washis washed with water
  5. dry with materialdried (Na2SO4)
  6. customevaporated
  7. customto give an oil which
  8. customcrystallizes from hexane