HRID253328

反应详情

EQUATION

反应方程式

HRID 253328 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 3.1 g of 2-fluoro-4-methyl-5-(2,2,2-trifluoroethylthio)phenylhydrazine, 1.9 g of trifluoroacetaldehyde ethyl hemiacetal, 0.5 g of methanesulfonic acid and 100 ml of ethanol was refluxed with heating for 5 hours. After the reaction mixture was cooled to room temperature, it was concentrated under reduced pressure and extracted with ethyl acetate, and the organic layer was dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure to obtain 3.7 g of trifluoroacetaldehyde {2-fluoro-4-methyl-5-(2,2,2-trifluoroethylthio)phenyl}hydrazone.

WORKUP

后处理

  1. temperaturewas refluxed
  2. temperaturewith heating for 5 hours
  3. concentrationit was concentrated under reduced pressure
  4. extractionextracted with ethyl acetate
  5. dry with materialthe organic layer was dried over anhydrous magnesium sulfate
  6. distillationThe solvent was distilled off under reduced pressure