HRID258325

反应详情

EQUATION

反应方程式

HRID 258325 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

13.9 g (0.128 mol) of α-fluoroacryloyl chloride (obtained in accordance with example 1c) were added dropwise, at a temperature of 25° C., with stirring and in the course of 30 minutes, to a solution of 30 g (0.0985 mol) of potassium pentachlorophenate in 400 ml of anhydrous acetonitrile, and the reaction mixture was then stirred for a further 90 minutes at the same temperature. The solid formed was filtered off and washed with 20 ml of anhydrous acetonitrile. After 0.01 g of hydroquinone monomethyl ether had been added, the volatile constituents in the mixture of filtrate and washing liquor were distilled off and the residue was recrystallized from boiling n-hexane. 17 g (51% of theory) of pentachlorophenyl α-fluoroacrylate were obtained, melting point 90° to 92° C.

WORKUP

后处理

  1. customThe solid formed
  2. filtrationwas filtered off
  3. washwashed with 20 ml of anhydrous acetonitrile
  4. additionAfter 0.01 g of hydroquinone monomethyl ether had been added
  5. additionthe volatile constituents in the mixture of filtrate
  6. washwashing liquor
  7. distillationwere distilled off
  8. customthe residue was recrystallized