HRID258327

反应详情

EQUATION

反应方程式

HRID 258327 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

27.5 g (0.169 mol) of 3-trifluoromethylphenol were dissolved in 100 ml of anhydrous methylene dichloride, and 17.1 g (0.169 mol) of triethylamine were added in portions to the solution; 20 g (0.184 mol) of α-fluoroacryloyl chloride (obtained in accordance with example 1c) were then added dropwise, at a temperature of 5° C., with stirring and in the course of 20 minutes, and the reaction mixture was stirred for a further 60 minutes at the same temperature. The solid formed was filtered off and washed with 30 ml of methylene dichloride. The mixture of filtrate and wash solution was distilled, after adding 0.01 g of hydroquinone monomethyl ether. 27 g (68% of theory) of 3-trifluoromethylphenyl α-fluoroacrylate were obtained, boiling point 78° to 79° C. (under 4 mbar).

WORKUP

后处理

  1. stirringthe reaction mixture was stirred for a further 60 minutes at the same temperature
  2. customThe solid formed
  3. filtrationwas filtered off
  4. washwashed with 30 ml of methylene dichloride
  5. additionThe mixture of filtrate
  6. washwash solution
  7. distillationwas distilled
  8. additionafter adding 0.01 g of hydroquinone monomethyl ether