反应详情

Into a mixture of 7.2 g of sodium hydride (60% in oil), 17.0 g of diethyl carbonate and 150 ml of tetrahydrofuran, 26.0 g of ethyl 2-chloro-6-fluorophenylacetate were added dropwise under heating, and then refluxed under heating for 8 hours. The reaction mixture was cooled, poured into iced dil. hydrochloric acid and extracted with t-butyl methyl ether. The organic layer was washed with water, dried over sodium sulfate and concentrated. The residue was subjected to silica gel column chromatography to give 30.4 g of diethyl (2-chloro-6-fluorophenyl)malonate.

1. additionwere added dropwise
2. temperatureunder heating
3. temperaturerefluxed
4. temperatureunder heating for 8 hours
5. temperatureThe reaction mixture was cooled
6. extractionextracted with t-butyl methyl ether
7. washThe organic layer was washed with water
8. dry with materialdried over sodium sulfate
9. concentrationconcentrated