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Diethyl Ether → 1-Bromo-3,3-dimethyl-4-fluoro-2-butanone

HRID 1447430
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HRID 1447430 반응식
[Br:1]Br.[CH3:3][C:4]([CH3:10])([CH2:8][F:9])[C:5](=[O:7])[CH3:6].CCOCC>O>[Br:1][CH2:6][C:5](=[O:7])[C:4]([CH3:10])([CH3:3])[CH2:8][F:9]
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참가 물질

5

반응물 3

HCID 3283Diethyl EtherHCID 24408BromineHCID 130194414-Fluoro-3,3-dimethylbutan-2-one

생성물 1

HCID 130194421-Bromo-3,3-dimethyl-4-fluoro-2-butanone수율 80%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

480 g of bromine were slowly added dropwise to a mixture of 354 g (3 mol) of 3,3-dimethyl-4-fluoro-2-butanone and 2,000 ml of ether at 20° C. to 30° C., while cooling and stirring. The yellowish solution was subsequently stirred for a further 1 hour at 20° C. and 500 ml of water were then carefully added. The ether phase was separated off, washed several times with water and dried over sodium sulphate. After distilling off the solvent, the residue was distilled under a waterpump vacuum. 472 g (80% of theory) of 1-bromo-3,3-dimethyl-4-fluoro-2-butanone of boiling point 80°-90° C./11 mm Hg were obtained. ##STR29##

후처리

  1. temperaturewhile cooling
  2. stirringThe yellowish solution was subsequently stirred for a further 1 hour at 20° C.
  3. customThe ether phase was separated off
  4. washwashed several times with water
  5. dry with materialdried over sodium sulphate
  6. distillationAfter distilling off the solvent
  7. distillationthe residue was distilled under a waterpump vacuum

출처 및 근거

ORD 기록
ord-e79b5873639947e59034f55d6f974859
출처 데이터셋
uspto-grants-1982_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04316910

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