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

HRID 851125
ノート
印刷プレビュー

反応式

HRID 851125 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-butan-2-one and 2,000 ml of ether at 20° to 30° C., while cooling and stirring. The yellowish solution was subsequently stirred, at 20° C., for a further 1 hour and 500 ml of water were then added carefully. 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% theory) of 1-bromo-3,3-dimethyl-4-fluoro-butan-2-one of boiling point 80°-90° C./11 mm Hg were obtained. ##STR24##

後処理

  1. temperaturewhile cooling
  2. stirringThe yellowish solution was subsequently stirred, at 20° C., for a further 1 hour
  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-cd9b21c646cb41da9b3e24b31e7fbd77
出典データセット
uspto-grants-1983_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04382944

反応ノート

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