تفاعل #1435737

معادلة التفاعل

tert-butyl methyl ether

sodium hydride

ethyl malonate

1-bromo-2,6-difluorobenzene

hydrochloric acid

→

diethyl (2,6-difluorophenyl)malonate

المذيبات

water

1,4-dioxane

ظروف التفاعل

المعالجة

1. 1
   workup.ADDITIONwere added dropwise at 60° C.
2. 2
   درجة الحرارةrefluxed for 16 hours
3. 3
   درجة الحرارةunder heating
4. 4
   درجة الحرارةcooling
5. 5
   غسيلThe separated organic layer was washed with dil. hydrochloric acid and water subsequently
6. 6
   تجفيفdried over sodium sulfate
7. 7
   تركيزconcentrated
8. 8
   workup.DISTILLATIONThe residue was distilled under reduced pressure

الإجراء التجريبي

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)

المصدر