反应 #2200627

ord-e109772573ec401c8cd74992df4e923f

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度The mixture was refluxed for 2 h
  2. 2
    其他the solvent was evaporated
  3. 3
    过滤The precipitate was filtered
  4. 4
    其他dried
  5. 5
    其他chromatographed (SiO2, heptanes:Ethyl acetate=100:0 to 80:2)

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]+.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07432256B2uspto-grants-2008_10