HRID1367481

反应详情

EQUATION

反应方程式

HRID 1367481 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a mixture of 4-bromo-2-trifluoromethyl-benzene sulfonyl chloride (9.38 g, 29 mmol) in dioxane (45 mL) and water (10 mL) was added tris-(2-carboxyethyl)phosphine hydrochloride (34.4 g, 118 mmol) and the reaction mixture was refluxed for 5 h, then cooled down, and partitioned between water and dichloromethane. The aqueous layer was extracted with dichloromethane and combined organic layers were washed with water then dried over sodium sulfate and concentrated in vacuo to afford the title compound (7.00 g, 94%) as a colorless liquid. MS (EI): 254.9 (M−H)−.

WORKUP

后处理

  1. temperaturethe reaction mixture was refluxed for 5 h
  2. temperaturecooled down
  3. custompartitioned between water and dichloromethane
  4. extractionThe aqueous layer was extracted with dichloromethane
  5. washwere washed with water
  6. dry with materialthen dried over sodium sulfate
  7. concentrationconcentrated in vacuo