HRID1786180

反应详情

EQUATION

反应方程式

HRID 1786180 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 3,3,3-trifluoro-propionic acid methyl ester (24.6 g, 173 mmol) in methanol (173 mL) was treated with hydrazine hydrate (8.4 mL, 173 mmol). The resulting mixture was then heated under reflux for 16 h and filtered. The filtrate was adsorbed on silica, evaporated and chromatographed (SiO2, dichloromethane:methanol=95:5 to 90:10). The title compound (14.2 g, 58%) was obtained as a white solid. MS: m/e=142.1 [M]+.

WORKUP

后处理

  1. temperatureThe resulting mixture was then heated
  2. temperatureunder reflux for 16 h
  3. filtrationfiltered
  4. customevaporated
  5. customchromatographed (SiO2, dichloromethane:methanol=95:5 to 90:10)