反应详情

Dissolve p-nitrophenol (11 g, 100 mmol), 3-chloropropanoic acid (14 g, 100 mmol) in a mixture of ethanol (100 mL) and 20% aqueous KOH solution (100 mL). Heat to reflux for 2 hrs, then adjust pH=1-3, extract with EtOAc (300 mL×3), combine the organic layers and wash with brine (300 mL×2), dry over anhydrous Na2SO4. Concentrate under reduced pressure to give the crude product. Purification by chromatography (silica gel, EtOAc:PE=1:4) affords the title compound (7.5 g, 14.9%). MS: (M+1): 212.1.

1. temperatureHeat
2. temperatureto reflux for 2 hrs
3. extractionextract with EtOAc (300 mL×3)
4. washwash with brine (300 mL×2)
5. dry with materialdry over anhydrous Na2SO4
6. concentrationConcentrate under reduced pressure
7. customto give the crude product
8. customPurification by chromatography (silica gel, EtOAc:PE=1:4)