HRID2264955

反应详情

EQUATION

反应方程式

HRID 2264955 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The 2-fluoro-4-trimethylsilylnitrobenzene (5.45 g, 25.6 mmol) was then dissolved in ethanol (100 mL), transferred to a Parr shaker bottle, flushed with nitrogen, then charged with 10% Pd—C (0.4 g). The reaction mixture was hydrogenated for 1 h on the Parr apparatus (45 psi H2), and then filtered through a plug of Celite. The filter cake was washed with ethanol, and the combined filtrates were concentrated. The resulting residue was purified by flash chromatography (250 mL silica gel, 95:5 hexane-ethyl ether), to afford the title compound as a tan oil (4.31 g, 92%).

WORKUP

后处理

  1. customflushed with nitrogen
  2. additioncharged with 10% Pd—C (0.4 g)
  3. filtrationfiltered through a plug of Celite
  4. washThe filter cake was washed with ethanol
  5. concentrationthe combined filtrates were concentrated
  6. customThe resulting residue was purified by flash chromatography (250 mL silica gel, 95:5 hexane-ethyl ether)