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Concentrated H2SO4 (1.5 ml) was added to a mixture of 3-amino-5-chloro-2-nitrobenzoic acid (70; 3.5 g, 16.2 mmol) in MeOH (120 ml). The resulting reaction mixture was stirred under reflux for 3 days. It was then neutralized with saturated aqueous Na2CO3 and extracted with EtOAc. The combined organic layers were dried (Na2SO4) and concentrated under reduced pressure. Purification by chromatography afforded methyl 3-amino-5-chloro-2-nitrobenzoate 71 (3.3 g, 88.5%) as a yellow solid.

1. customThe resulting reaction mixture
2. temperatureunder reflux for 3 days
3. extractionextracted with EtOAc
4. dry with materialThe combined organic layers were dried (Na2SO4)
5. concentrationconcentrated under reduced pressure
6. customPurification by chromatography