반응 #1435737

반응 방정식

tert-butyl methyl ether

sodium hydride

ethyl malonate

1-bromo-2,6-difluorobenzene

hydrochloric acid

→

diethyl (2,6-difluorophenyl)malonate

용매

water

1,4-dioxane

반응 조건

후처리

1. 1
   workup.ADDITIONwere added dropwise at 60° C.
2. 2
   온도refluxed for 16 hours
3. 3
   온도under heating
4. 4
   온도cooling
5. 5
   세척The separated organic layer was washed with dil. hydrochloric acid and water subsequently
6. 6
   건조dried over sodium sulfate
7. 7
   농축concentrated
8. 8
   workup.DISTILLATIONThe residue was distilled under reduced pressure

실험 절차

Into a mixture of 8.00 g of sodium hydride (60% in oil) and 100 ml of 1,4-dioxane, 32.0 g of ethyl malonate were added dropwise at 60° C. , further 14.6 g of cuprous bromide and 19.3 g of 1-bromo-2,6-difluorobenzene were added subsequently, and then refluxed for 16 hours under heating. To the reaction mixture, conc. hydrochloric acid was added under ice-cooling, and then tert-butyl methyl ether and water were added. The separated organic layer was washed with dil. hydrochloric acid and water subsequently, dried over sodium sulfate and concentrated. The residue was distilled under reduced pressure to give 16.5 g of diethyl (2,6-difluorophenyl)malonate. b.p. 107–109° C. (0.14 mmHg)

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