HRID1697620

反应详情

EQUATION

反应方程式

HRID 1697620 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

4-Fluoro-2-(trifluoromethyl)benzenesulphonyl chloride (2 g) was dissolved in 1,4-dioxane (12 mL) and water (3 mL) under a nitrogen atmosphere. Tris-(2-carboxylethyl)phosphine hydrochloride (8.73 g) was added and the mixture was stirred under reflux for 6 h. The reaction mixture was cooled to 25° C. and water (20 mL) was added. The product was extracted 3 times with CH2Cl2 (20 mL). The combined organic layers were dried over Na2SO4 filtrated and evaporated to dryness to yield the title compound (1.27 g, 85%) as a colorless liquid. MS (ESI): m/z=194.9 [M−H]−.

WORKUP

后处理

  1. temperatureunder reflux for 6 h
  2. extractionThe product was extracted 3 times with CH2Cl2 (20 mL)
  3. dry with materialThe combined organic layers were dried over Na2SO4
  4. filtrationfiltrated
  5. customevaporated to dryness