HRID1514873

反应详情

EQUATION

反应方程式

HRID 1514873 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-m-xylene (1.51 g) and 10% Pd/C (80 mg) in MeOH (50 mL) was stirred at room temperature under H2 balloon for 16 h. The reaction mixture was filtered through a Celite pad, washed with EtOAc, concentrated under reduced pressure. The crude product was purified by column chromatography (SiO2, EtOAc:Hexane=5:95 to 40:60) to give 3,5-dimethyl-phenylamine as a yellow oil: MS (m/z) 122 (M+1); 1H NMR (CDCl3, 400 MHz) δ 6.41 (s, 1H), 6.33 (s, 2H), 3.52 (s, 2H), 2.22 (s, 6H).

WORKUP

后处理

  1. filtrationThe reaction mixture was filtered through a Celite pad
  2. washwashed with EtOAc
  3. concentrationconcentrated under reduced pressure
  4. customThe crude product was purified by column chromatography (SiO2, EtOAc:Hexane=5:95 to 40:60)