HRID273972

反应详情

EQUATION

反应方程式

HRID 273972 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-65 °C

PROCEDURE

实验过程

Inside of a 100 ml volume glass three-neck flask equipped with a 50 mol volume glass dropping funnel, temperature resistor and septum rubber was sufficiently replaced with nitrogen. Into the flask, 5 g (29.8 mmol) of pentafluorobenzene and 30 ml of diethyl ether were charged, of which solution was cooled to -65° C. Thereafter, 14.2 g (34.3 mmol) of 15.5 wt. % hexane solution of sec-butyllithium charged into the dropping funnel were added dropwise while making the inner temperature not to exceed -55° C. After the completion of dropwise addition, the reaction mixture was kept at a temperature of -65°~-55° C. with stirring to give pentafluorophenyllithium. The yield of pentafluorobenzoic acid obtained by blowing of carbon dioxide into the prepared solution of pentafluorophenyllithium was 96.8% by means of gas chromatographic quantitative determination.

WORKUP

后处理

  1. customInside of a 100 ml volume glass three-neck flask equipped with a 50 mol volume glass
  2. additionwere added dropwise
  3. customto exceed -55° C
  4. additionAfter the completion of dropwise addition
  5. customwas kept at a temperature of -65°~-55° C.