1-(4-(Hydroxymethyl)phenyl)ethanone → 2-Bromo-1-[4-(hydroxymethyl)phenyl]ethanone

HRID 564063ノート

反応式

HRID 564063 の反応式
[OH:1][CH2:2][C:3]1[CH:8]=[CH:7][C:6]([C:9](=[O:11])[CH3:10])=[CH:5][CH:4]=1.[Br-:12].[Br-].[Br-].C([N+](CCCC)(CCCC)CCCC)CCC.C([N+](CCCC)(CCCC)CCCC)CCC.C([N+](CCCC)(CCCC)CCCC)CCC>C1COCC1.CO.C1COCC1>[Br:12][CH2:10][C:9]([C:6]1[CH:7]=[CH:8][C:3]([CH2:2][OH:1])=[CH:4][CH:5]=1)=[O:11]

参加物

5

反応物 2

HCID 5852641-(4-(Hydroxymethyl)phenyl)ethanoneHCID 23500184Tetra-n-butylammonium tribromide

生成物 1

HCID 197980532-Bromo-1-[4-(hydroxymethyl)phenyl]ethanone

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒HCID 21899815MeOH tetrahydrofuran溶媒

実験手順

To 7.00 g (46.6 mmol) 1-(4-hydroxymethyl-phenyl)-ethanone in 100 mL THF is added 22.5 g (46.6 mmol) tetrabutylammonium-tribromide dissolved in MeOH/THF. The reaction mixture is stirred 1 h at RT and the solvent is evaporated. The residue is dissolved with water and tertbutylmethylether. The organic phase is washed eight times with water. The combined organic phase is dried over MgSO4, filtered and the solvent is evaporated. The residue is elutriated with diisopropylether and the precipitate is collected and dried.

後処理

  1. customthe solvent is evaporated
  2. dissolutionThe residue is dissolved with water and tertbutylmethylether
  3. washThe organic phase is washed eight times with water
  4. dry with materialThe combined organic phase is dried over MgSO4
  5. filtrationfiltered
  6. customthe solvent is evaporated
  7. customthe precipitate is collected
  8. customdried

出典と根拠

ORDレコード
ord-8fab9a1e59cc4af5bde38fab9d368b85
出典データセット
uspto-grants-2011_11
特許番号
US08067590B2

反応ノート

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