HRID1786219

反应详情

EQUATION

反应方程式

HRID 1786219 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 2-fluoro-5-trifluoromethoxy-benzaldehyde (9.78 g, 47 mmol) in ethanol (50 mL) was treated with hydroxylamine HCl (3.59 g, 52 mmol) and sodium acetate (4.27 g, 52 mmol). The resulting mixture was heated under reflux for 2 h. The solvent was then evaporated and the residue stirred with water (50 mL). The precipitate was filtered off, dried and chromatographed (SiO2, heptanes:ethyl acetate=100:0 to 80:2) to afford the title compound (9.21 g, 88%) as a white solid. MS: m/e=223.0 [M]+.

WORKUP

后处理

  1. temperatureThe resulting mixture was heated
  2. temperatureunder reflux for 2 h
  3. customThe solvent was then evaporated
  4. filtrationThe precipitate was filtered off
  5. customdried
  6. customchromatographed (SiO2, heptanes:ethyl acetate=100:0 to 80:2)