Reaktion #1435737

Reaktionsgleichung

tert-butyl methyl ether

sodium hydride

ethyl malonate

1-bromo-2,6-difluorobenzene

hydrochloric acid

→

diethyl (2,6-difluorophenyl)malonate

Lösungsmittel

water

1,4-dioxane

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONwere added dropwise at 60° C.
2. 2
   Temperaturrefluxed for 16 hours
3. 3
   Temperaturunder heating
4. 4
   Temperaturcooling
5. 5
   WaschenThe separated organic layer was washed with dil. hydrochloric acid and water subsequently
6. 6
   Trocknendried over sodium sulfate
7. 7
   Einengenconcentrated
8. 8
   workup.DISTILLATIONThe residue was distilled under reduced pressure

Vorschrift

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)

Quelle