HRID1022405

反应详情

EQUATION

反应方程式

HRID 1022405 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 762 mg of 2-amino-5-trifluoromethylbenzophenone in 10 ml of chloroform was added dropwise 349 mg of triethylamine, and then 627 mg of trichloroacetyl chloride was added dropwise under ice-cooling. After stirring at the same temperature for 30 minutes, 50 ml of water was added, thereby separating the solution. The organic layer was collected and then concentrated. The resulting residue was purified by silica gel column chromatography (hexane:ethyl acetate=5:1) to obtain 1.08 g of 2′-benzoyl-2,2,2-trichloro-4′-trifluoromethylacetanilide. 1H NMR (CDCl3): 7.53-7.58 (2H, m), 7.66-7.75 (3H, m), 7.90-7.95 (2H, m), 8.81 (1H, d, J=8.6 Hz), 12.38 (1H, br. s).

WORKUP

后处理

  1. temperaturecooling
  2. customseparating the solution
  3. customThe organic layer was collected
  4. concentrationconcentrated
  5. customThe resulting residue was purified by silica gel column chromatography (hexane:ethyl acetate=5:1)