反应详情

A solution of dimethyl 2-(2-chloro-5-methoxy-4-nitrophenyl)malonate (15.5 g, 48.7 mmol), sodium chloride (5.70 g, 97.5 mmol) and water (0.876 mL, 48.7 mmol) in DMSO (200 mL) was heated to 120° C. for 2 hours. The cooled reaction mixture was partitioned between water (1000 mL) and EtOAc (200 mL) and the separated aqueous phase was extracted with EtOAc (200 mL). The combined organic extracts were washed with brine (150 mL), dried (Na2SO4) and concentrated under reduced pressure. The crude product was purified by column chromatography on neutral silica gel using 3-10% EtOAc in hexane to give the title compound (10.2 g, 86%) as a solid.

1. customThe cooled reaction mixture
2. customwas partitioned between water (1000 mL) and EtOAc (200 mL)
3. extractionthe separated aqueous phase was extracted with EtOAc (200 mL)
4. washThe combined organic extracts were washed with brine (150 mL)
5. dry with materialdried (Na2SO4)
6. concentrationconcentrated under reduced pressure
7. customThe crude product was purified by column chromatography on neutral silica gel using 3-10% EtOAc in hexane