HRID2113445

反应详情

EQUATION

反应方程式

HRID 2113445 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 mixture was refluxed for 2 h, the solvent was evaporated and the residue stirred with water (50 ml). The precipitate was filtered, dried and chromatographed (SiO2, heptanes:Ethyl acetate=100:0 to 80:2) and afforded the title compound (9.21 g, 88%) as a white solid. MS: m/e=223.0 [M]+.

WORKUP

后处理

  1. temperatureThe mixture was refluxed for 2 h
  2. customthe solvent was evaporated
  3. filtrationThe precipitate was filtered
  4. customdried
  5. customchromatographed (SiO2, heptanes:Ethyl acetate=100:0 to 80:2)