反应详情

温度

80 °C

To a suspension of NaH (60% in oil, 1.4 g, 36 mmol)) in DMF (50 mL) was added tert-butyl ethyl propanedioate (6.8 g, 36 mmol) at room temperature. The mixture was stirred for 30 min. A solution of 3-chloro-2-methyl-6-nitropyridine (4.8 g, 28 mmol) in DMF (10 mL) was added. The mixture was heated to 80° C. and stirred for 5 h. Cooled to ambient temperature, poured to ice/water, extracted with EtOAc. The combined organic layer was washed with brine, dried over anhydrous Na2SO4, concentrated and the residue was purified by column chromatography to give title compound.

1. stirringstirred for 5 h
2. temperatureCooled to ambient temperature
3. extractionextracted with EtOAc
4. washThe combined organic layer was washed with brine
5. dry with materialdried over anhydrous Na2SO4
6. concentrationconcentrated
7. customthe residue was purified by column chromatography