反应详情

Acetyl chloride (35.2 mmol, 2.5 mL) was added dropwise to a stirring solution of 4-amino-2-chloro-benzoic acid 70l (12.9 mmol, 2.22 g) in methanol (50 mL). The mixture was heated at reflux for 18 h, cooled, and concentrated under vacuum. The residue was taken up in EtOAc, washed with saturated aqueous NaHCO3 and brine, dried, and concentrated under vacuum. The crude product was purified by flash column chromatography (silica gel, 30% EtOAc/hexanes) to give compound 70m.

1. temperatureThe mixture was heated
2. temperatureat reflux for 18 h
3. temperaturecooled
4. concentrationconcentrated under vacuum
5. washwashed with saturated aqueous NaHCO3 and brine
6. customdried
7. concentrationconcentrated under vacuum
8. customThe crude product was purified by flash column chromatography (silica gel, 30% EtOAc/hexanes)