HRID391377

反应详情

EQUATION

反应方程式

HRID 391377 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

(3-Nitro-5-(trifluoromethyl)phenyl)methanol (2.6 g, 11.6 mmol) in methanol (30 mL) was flushed with nitrogen, and treated with palladium (10% on charcoal, 260 mg). The flask was flushed with hydrogen and allowed to stir under an atmosphere of hydrogen overnight. The reaction was flushed with nitrogen, filtered through celite, and concentrated. Column chromatography on silica gel (50% ethyl acetate/hexanes) afforded 1.9 g (85%). 1H-NMR (CDCl3, 500 MHz) δ 6.95 (s, 1H), 6.80 (s, 1H), 6.79 (s, 1H), 4.61 (s, 2H). Mass spec.: 192.15 (MH)+.

WORKUP

后处理

  1. customThe flask was flushed with hydrogen
  2. customThe reaction was flushed with nitrogen
  3. filtrationfiltered through celite
  4. concentrationconcentrated
  5. customColumn chromatography on silica gel (50% ethyl acetate/hexanes) afforded 1.9 g (85%)