HRID1293295

反应详情

EQUATION

反应方程式

HRID 1293295 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A suspension of methyl 2-(2,6-difluorophenoxy)-5-nitrobenzoate (step 1, 365 mg, 1.18 mmol) and 5% Pd/C (37 mg) in methanol (10 mL) was stirred under hydrogen atmosphere for 16 h at room temperature. After filtration through a pad of Celite®, the filtrate was concentrated. The residue was purified by column chromatography on silica gel eluting with hexane/ethyl acetate (5/1 to 1/2) to afford 325 mg of the title compound: 1H-NMR (CDCl3) δ 7.21 (1H, d, J=2.9 Hz), 7.12–6.88 (3H, m), 6.77 (1H, dd, J=8.8, 2.9 Hz), 6.64–6.58 (1H, m), 3.87 (3H, s).

WORKUP

后处理

  1. filtrationAfter filtration through a pad of Celite®
  2. concentrationthe filtrate was concentrated
  3. customThe residue was purified by column chromatography on silica gel eluting with hexane/ethyl acetate (5/1 to 1/2)