HRID1510237

反应详情

EQUATION

反应方程式

HRID 1510237 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a refluxing mixture of 3-fluoro-4-(4-nitrophenyl)pyridine (2.23 g), trichloroiron (130 mg) and activated carbon (1.12 g, 50 wt % of the starting material) in ethanol (74 mL) was added dropwise hydrazine hydrate (1.6 g), and the mixture was stirred for 3 hours. The insoluble materials were removed by filtration in hot and washed with ethanol. Most of ethanol was removed in vacuo, and to the residue was added water. Resulting solid was collected by filtration, and purified by column chromatography on silica gel eluting with hexane/ethyl acetate (1:2) to afford 4-(3-fluoropyridin-4-yl)aniline (1.36 g) a pale orange solid.

WORKUP

后处理

  1. customThe insoluble materials were removed by filtration in hot and
  2. washwashed with ethanol
  3. customMost of ethanol was removed in vacuo
  4. additionto the residue was added water
  5. customResulting solid
  6. filtrationwas collected by filtration
  7. custompurified by column chromatography on silica gel eluting with hexane/ethyl acetate (1:2)