反应详情

To a suspension of prewashed sodium hydride (76.8 g) in ether was added 189 g of diethylcarbonate. The mixture was heated to reflux and a solution of 131.84 g of 6-acetyl-1,3-dichloro-4-fluorobenzene in 1500 ml of ether was added dropwise over 5 hours. The mixture was then refluxed 24 hours, cooled, poured onto a mixture of ice and acetic acid and extracted several times with ether. The ether extracts were combined, washed with water, dried and evaporated. The residue was purified by vacuum distillation giving 80 g of ethyl 2,4-dichloro-5-fluorobenzoylacetate.

1. temperatureThe mixture was heated
2. temperatureto reflux
3. temperatureThe mixture was then refluxed 24 hours
4. temperaturecooled
5. extractionextracted several times with ether
6. washwashed with water
7. customdried
8. customevaporated
9. distillationThe residue was purified by vacuum distillation