HRID1272732

反应详情

EQUATION

反应方程式

HRID 1272732 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A suspension of 5-nitro-3-phenyl-1H-indazole (0.239 g, 1.0 mmol) and palladium (10 wt % on activated carbon, 30 mg) in ethyl acetate (10 mL) was stirred under hydrogen at ambient temperature for 18 hours. It was filtered with celite and washed with ethyl acetate. The filtrate was concentrated and the residue was then purified by chromatography (SiO2, 30–50% ethyl acetate/hexane) to provide the title compound (0.184 g, 88% yield): mp 104° C.; 1H NMR (CDCl3) δ 10.40 (br s, 1H), 7.94 (d, 2H), 7.51 (m, 2H), 7.20–7.42 (m, 3H), 6.90 (m, 1H), 3.6 (br, 2H); EI-MS (m/z) 209 [M]+.

WORKUP

后处理

  1. filtrationIt was filtered with celite
  2. washwashed with ethyl acetate
  3. concentrationThe filtrate was concentrated
  4. customthe residue was then purified by chromatography (SiO2, 30–50% ethyl acetate/hexane)