反应详情

温度

60 °C

To a suspension of methyl 5-cyano-2-hydroxy-benzoate (ASTATECH; 63806; 1 g; 5.64 mmol; 1 eq.) in EtOH (10 mL) was added hydroxylamine (50% in water) (1.69 mL; 28.22 mmol; 5 eq.). The reaction mixture was stirred at 60° C. for 30 min. While cooling to RT a white precipitate was formed. Solvents were removed to dryness and the white solids were washed with EtOH to afford title compound pure at 66% as a white powder. 1H NMR (DMSO-d6, 300 MHz) δ 8.12 (d, J=2.2 Hz, 1H), 7.81 (dd, J=8.4, 2.2 Hz, 1H), 6.99 (d, J=8.7 Hz, 1H), 5.82 (br s, 2H), 5.69 (br s, 1H), 3.91 (s, 3H). LC/MS (Method A): 210.8 (M+H)+.

1. temperatureWhile cooling to RT a white precipitate
2. customwas formed
3. customSolvents were removed to dryness
4. washthe white solids were washed with EtOH