反应详情

To a stirred solution of 2-amino-4-methoxy-benzoic acid (3.00 g, 17.9 mmol) in THF (90 mL), EDCl (7.89 g, 41.1 mmol) and HOBt (7.95 g, 51.9 mmol) were added and stirred at room temperature for 30 minutes. Then, N-methylmorpholine (6.15 g, 60.0 mmol) and aqueous 50% (v/v) NH4OH (12 mL, 171.4 mmol) were added. The mixture was stirred for 16 hours at room temperature. The solvent was removed under reduced pressure and the residue was extracted with ethyl acetate (4×100 mL). The combined organic phase was washed with water, then brine, and dried over anhydrous sodium sulfate. Solvent was evaporated to give 2-amino-4-methoxy-benzamide as an off-white solid. Yield: 1.80 g, (60%).

1. stirringThe mixture was stirred for 16 hours at room temperature
2. customThe solvent was removed under reduced pressure
3. extractionthe residue was extracted with ethyl acetate (4×100 mL)
4. washThe combined organic phase was washed with water
5. dry with materialbrine, and dried over anhydrous sodium sulfate
6. customSolvent was evaporated