반응 #1435727

반응 방정식

hydrochloric acid

sodium hydride

diethyl carbonate

ethyl 2-chloro-6-fluorophenylacetate

→

diethyl (2-chloro-6-fluorophenyl)malonate

수율 87.7%

용매

tetrahydrofuran

반응 조건

후처리

1. 1
   workup.ADDITIONwere added dropwise
2. 2
   온도under heating
3. 3
   온도refluxed
4. 4
   온도under heating for 8 hours
5. 5
   온도The reaction mixture was cooled
6. 6
   추출extracted with t-butyl methyl ether
7. 7
   세척The organic layer was washed with water
8. 8
   건조dried over sodium sulfate
9. 9
   농축concentrated

실험 절차

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.

출처