反应详情

To a solution of 3-methoxy-4-nitrobenzoic acid (5.0 g, 25.4 mmol) and N1,N1-dimethylethane-1,2-diamine (2.7 g, 30.5 mmol) in dichloromethane (200 mL) were added 1-hydroxybenzotriazole hydrate (7.8 g, 50.8 mmol), 1-ethyl-(3-dimethyl aminopropyl)carbodiimide hydrochloride (9.7 g, 50.8 mmol) and N,N-diisopropyl ethylamine (13.1 g, 101.6 mmol) and the mixture was stirred at ambient temperature for 16 hours. The mixture was washed with water (50 mL), dried over sodium sulfate, filtered, and concentrated. The residue was purified by flash chromatography on silica gel (200-300 mesh) eluting with 20/1 dichloromethane/methanol to give the title compound. MS: 268 (M+H+).

1. washThe mixture was washed with water (50 mL)
2. dry with materialdried over sodium sulfate
3. filtrationfiltered
4. concentrationconcentrated
5. customThe residue was purified by flash chromatography on silica gel (200-300 mesh)
6. washeluting with 20/1 dichloromethane/methanol