反应详情

To 5-hydroxy-2-nitrobenzaldehyde (1.0 g, 6.0 mmol) in 2.5M NaOH(aq) (10 mL) at 100° C. was added 35% H2O2 (12 mL) dropwise over 10 minutes and the mixture heated at reflux overnight. The solution was acidified with 10% H2SO4, extracted with EtOAc (2×100 mL), and the combined organic layers washed with H2O and brine, dried over MgSO4, filtered and concentrated in vacuo to give 5-hydroxy-2-nitrobenzoic acid (1.03 g, 5.63 mmol, 94%). LC-MS (ESI) m/z 182 (M−H)+.

1. temperaturethe mixture heated
2. temperatureat reflux overnight
3. extractionextracted with EtOAc (2×100 mL)
4. washthe combined organic layers washed with H2O and brine
5. dry with materialdried over MgSO4
6. filtrationfiltered
7. concentrationconcentrated in vacuo