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

HRID 530418

反応式

HRID 530418 の反応式
[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]

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 74236Tetrabutylammonium Bromide触媒HCID 6228Dimethylformamide溶媒

反応条件

温度
130 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-db3d9c4942684569a92fbb51e49d6c6c
出典データセット
uspto-grants-2016_05
特許番号
US09353089B2

関連ノート

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