Hydrogen Peroxide → 5-Hydroxy-2-nitrobenzoic acid

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Reaction Steps

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)+.

Provenance & Evidence