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

HRID 564063노트

반응식

HRID 564063 반응식
[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]

참가 물질

5

반응물 2

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

생성물 1

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

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매HCID 21899815MeOH tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-8fab9a1e59cc4af5bde38fab9d368b85
출처 데이터셋
uspto-grants-2011_11
특허 번호
US08067590B2

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