HRID1886560

反应详情

EQUATION

反应方程式

HRID 1886560 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
10 °C

PROCEDURE

实验过程

157 g (0.96 mole) of 2-tert-butyl-6-methylaniline are added dropwise to 500 ml of 40% strength tetrafluoroboric acid at 50° C., followed by a solution of 66.2 g (0.96 mole) of sodium nitrite in 270 ml of water. The mixture is stirred for 1 hour at 10° C. The precipitated diazonium salt is filtered off under suction, washed in succession with 50 ml of ice water, 50 ml of cold ethanol and 50 ml of diethyl ether and then suspended in 500 ml of liquid paraffin. The suspension is then added dropwise to a flask preheated at 150° C. After evolution of gas is ended, the product is obtained by distillation over a Claisen still (bath temperature 140° C., pressure 26 mbar) at a distillation temperature of 83° C. 47 g (29%) of 2-fluoro-3-tert-butyltoluene are obtained.

WORKUP

后处理

  1. filtrationThe precipitated diazonium salt is filtered off under suction
  2. washwashed in succession with 50 ml of ice water, 50 ml of cold ethanol and 50 ml of diethyl ether
  3. additionThe suspension is then added dropwise to a flask
  4. custompreheated at 150° C
  5. customthe product is obtained by distillation over a Claisen still (bath temperature 140° C., pressure 26 mbar) at a distillation temperature of 83° C