反应详情

温度

120 °C

A mixture of dimethyl 2-(2-chloro-5-methoxy-4-nitrophenyl)malonate (3.0 g, 9.44 mmol) and sodium chloride (0.99 g, 16.99 mmol) in DMSO (50 mL) and water (0.17 mL, 9.44 mmol) was heated for 5 hours at 120° C. The reaction mass was allowed to cool to room temperature and water (400 mL) and EtOAc (50 mL) were added and stirring continued for 15 minutes. The separated aqueous layer was extracted with EtOAc (50 mL), and then the combined organic layers were washed with brine (50 mL), dried (Na2SO4) and concentrated under reduced pressure. The crude residue was purified by column chromatography on neutral silica gel using 15-25% EtOAc in hexane to give the desired material (1.5 g, 61%) as a solid.

1. temperatureto cool to room temperature
2. extractionThe separated aqueous layer was extracted with EtOAc (50 mL)
3. washthe combined organic layers were washed with brine (50 mL)
4. dry with materialdried (Na2SO4)
5. concentrationconcentrated under reduced pressure
6. customThe crude residue was purified by column chromatography on neutral silica gel using 15-25% EtOAc in hexane