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

HRID 1447430
ノート
印刷プレビュー

反応式

HRID 1447430 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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##

後処理

  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

出典と根拠

ORDレコード
ord-e79b5873639947e59034f55d6f974859
出典データセット
uspto-grants-1982_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04316910

反応ノート

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