HRID1030440

反应详情

EQUATION

反应方程式

HRID 1030440 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

406 grams of (3.08 mo) 2,2,3,3-tetrafluoropropanol, 613 gm (3.22 mol) tosyl chloride, and 1200 ml water were heated to 50° C. with mechanical stirring. Sodium hydroxide (139.7 gm, 3.5 ml) in 560 ml water was added at a rate such that the temperature remained less than 65° C. After the addition was completed, the mixture was stirred at 50° C. until the pH of the aqueous phase was 6. The mixture was cooled and extracted with 1.5 liters methylene chloride. The organic layer was washed twice with 200 ml aqueous ammonia, 350 ml water, dried with magnesium sulfate, and distilled to give 697.2 gm (79%) viscous oil.

WORKUP

后处理

  1. customremained less than 65° C
  2. additionAfter the addition
  3. temperatureThe mixture was cooled
  4. extractionextracted with 1.5 liters methylene chloride
  5. washThe organic layer was washed twice with 200 ml aqueous ammonia, 350 ml water
  6. dry with materialdried with magnesium sulfate
  7. distillationdistilled