HRID1293295
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
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
- filtrationAfter filtration through a pad of Celite®
- concentrationthe filtrate was concentrated
- customThe residue was purified by column chromatography on silica gel eluting with hexane/ethyl acetate (5/1 to 1/2)