HRID1649523

反应详情

EQUATION

反应方程式

HRID 1649523 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 72 g of N-methyl-2-nitrobenzenesulfonamide, 35 g of tetrafluoroethylene and 4 g of powdered potassium hydroxide in 150 ml of dimethylformamide was heated at 85° for 3 hours in a pressure vessel. The reaction mixture was cooled to 25° and poured into 800 ml of water. A heavy oil was separated and the aqueous layer extracted with 150 ml of 1-chlorobutane. The heavy oil, the 1-chlorobutane extract and an additional 300 ml of 1-chlorobutane were combined and washed three times with water. The organic solution was dried over magnesium sulfate and concentrated in-vacuo to yield 85.1 g of N-methyl-N-(1,1,2,2-tetrafluoroethyl)-2-nitrobenzenesulfonamide as a viscous orange oil.

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled to 25°
  2. customA heavy oil was separated
  3. extractionthe aqueous layer extracted with 150 ml of 1-chlorobutane
  4. extractionThe heavy oil, the 1-chlorobutane extract
  5. washwashed three times with water
  6. dry with materialThe organic solution was dried over magnesium sulfate
  7. concentrationconcentrated in-vacuo