Реакция #1435737

Уравнение реакции

tert-butyl methyl ether

sodium hydride

ethyl malonate

1-bromo-2,6-difluorobenzene

hydrochloric acid

→

diethyl (2,6-difluorophenyl)malonate

Растворители

water

1,4-dioxane

Условия реакции

Обработка

1. 1
   workup.ADDITIONwere added dropwise at 60° C.
2. 2
   Температураrefluxed for 16 hours
3. 3
   Температураunder heating
4. 4
   Температураcooling
5. 5
   ПромывкаThe separated organic layer was washed with dil. hydrochloric acid and water subsequently
6. 6
   Сушкаdried over sodium sulfate
7. 7
   Концентрированиеconcentrated
8. 8
   workup.DISTILLATIONThe residue was distilled under reduced pressure

Методика

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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