HRID74021

反应详情

EQUATION

反应方程式

HRID 74021 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 4,6-di-tert-butyl-3-nitrobenzene-1,2-diol (1.92 g, 7.2 mmol) in EtOH (70 mL) was added Pd-5% wt. on carbon (200 mg). The mixture was stirred under H2 (1 atm) for 2 h. The reaction was recharged with Pd-5% wt. on carbon (200 mg) and stirred under H2 (1 atm) for another 2 h. The mixture was filtered through Celite and the filtrate was concentrated and purified by column chromatography (10-40% ethyl acetate-hexanes) to give 4,6-di-tert-butyl-3-aminobenzene-1,2-diol (C-26) (560 mg, 33%). 1H NMR (400 MHz, CDCl3) δ 7.28 (s, 1H), 1.42 (s, 9H), 1.38 (s, 9H).

WORKUP

后处理

  1. stirringstirred under H2 (1 atm) for another 2 h
  2. filtrationThe mixture was filtered through Celite
  3. concentrationthe filtrate was concentrated
  4. custompurified by column chromatography (10-40% ethyl acetate-hexanes)