反应详情

温度

100 °C

Sodium hydride (504 mg, 12.6 mmol) was added portionwise to an ice bath chilled solution of benzyl ethyl malonate (2.9 g, 12.6 mmol) in dry DMF (20 ml) and stirred for 10 minutes. At room temperature 3,4-difluoronitrobenzene (2 g, 12.6 mmol) was added and stirred under argon. Heated at 100° C. for 20 hours. The reaction mixture was cooled and partitioned between 2N Hydrochloric acid (75 ml) and ethyl acetate (75 ml). The aqueous layer was extracted with ethyl acetate (2×75 ml) and the combined organics were evaporated to a yellow oil. Purified by chromatography on silica gel eluting with ethyl acetate/hexane (1:4) to give the title compound as a yellow oil (3.86 g, 10.6 mmol). LC/MS: Rt=3.40, [MH]+ 362

1. stirringstirred under argon
2. temperatureThe reaction mixture was cooled
3. custompartitioned between 2N Hydrochloric acid (75 ml) and ethyl acetate (75 ml)
4. extractionThe aqueous layer was extracted with ethyl acetate (2×75 ml)
5. customthe combined organics were evaporated to a yellow oil
6. customPurified by chromatography on silica gel eluting with ethyl acetate/hexane (1:4)