HRID2307422

反应详情

EQUATION

反应方程式

HRID 2307422 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2,2,2-trifluoro-1-(3-nitro-phenyl)ethanone (4 g), NH2OH.HCl (5.037 g), and Et3N (20.44 g) in EtOH (80 mL) was refluxed for 4 days. After concentration, the residue was extracted with CH2Cl2. The organic layer was washed with water and dried over MgSO4. The crude product was purified by silica gel flash chromatography (30% ethyl acetate in hexanes) to give the title compound (3.4 g) as a solid.

WORKUP

后处理

  1. temperaturewas refluxed for 4 days
  2. concentrationAfter concentration
  3. extractionthe residue was extracted with CH2Cl2
  4. washThe organic layer was washed with water
  5. dry with materialdried over MgSO4
  6. customThe crude product was purified by silica gel flash chromatography (30% ethyl acetate in hexanes)