1-Bromo-2-methylpropane → 1,2-Bis(4-isobutoxyphenyl)ethane-1,2-dione

HRID 530418

반응식

HRID 530418 반응식
[OH:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](=[O:18])[C:9]([C:11]2[CH:16]=[CH:15][C:14]([OH:17])=[CH:13][CH:12]=2)=[O:10])=[CH:4][CH:3]=1.C(=O)([O-])[O-].[K+].[K+].Br[CH2:26][CH:27]([CH3:29])[CH3:28]>CN(C=O)C.[Br-].C([N+](CCCC)(CCCC)CCCC)CCC>[CH2:26]([O:1][C:2]1[CH:3]=[CH:4][C:5]([C:8](=[O:18])[C:9]([C:11]2[CH:16]=[CH:15][C:14]([O:17][CH2:4][CH:5]([CH3:8])[CH3:6])=[CH:13][CH:12]=2)=[O:10])=[CH:6][CH:7]=1)[CH:27]([CH3:29])[CH3:28]

참가 물질

6

반응물 3

HCID 65551-Bromo-2-methylpropaneHCID 11430Potassium CarbonateHCID 4582044,4'-Dihydroxybenzil

생성물 1

HCID 1176004381,2-Bis(4-isobutoxyphenyl)ethane-1,2-dione수율 212.9%

시약·촉매·용매 2

HCID 74236Tetrabutylammonium Bromide촉매HCID 6228Dimethylformamide용매

반응 조건

온도
130 °C

실험 절차

1,2-Bis(4-hydroxyphenyl)ethane-1,2-dione (0.77 g, 3.18 mmol) was dissolved in 20 mL of DMF. Potassium carbonate (1.3 g, 9.4 mmol), tetrabutylammonium bromide (0.5 g, 1.55 mmol) and 1-bromo-2-methylpropane (0.86 mL, 7.91 mmol) were added, then the reaction was stirred at 130° C. overnight. The mixture was extracted with ethyl acetate and the organic phase was washed with water, dried over sodium sulfate. Concentration under vacuum gave the title compound as oil (1.2 g, quantitative).

후처리

  1. extractionThe mixture was extracted with ethyl acetate
  2. washthe organic phase was washed with water
  3. dry with materialdried over sodium sulfate
  4. concentrationConcentration under vacuum

출처 및 근거

ORD 기록
ord-db3d9c4942684569a92fbb51e49d6c6c
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09353089B2

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