Ethanol → HCID 10633568、化合物

HRID 565848ノート

反応式

HRID 565848 の反応式
B([O-])([O-])O[C:3]1[CH:8]=[CH:7][C:6]([CH3:9])=[CH:5][CH:4]=1.[C:12](=[O:15])([O-])[O-].[K+].[K+].[C:18]1([CH3:24])[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1.[CH2:25](O)[CH3:26]>C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.O>[CH3:24][C:18]1[CH:23]=[CH:22][C:21]([C:3]2[CH:8]=[C:7]3[C:6]([CH2:9][CH2:25][CH2:26][C:12]3=[O:15])=[CH:5][CH:4]=2)=[CH:20][CH:19]=1

参加物

7

反応物 4

HCID 702EthanolHCID 1140TolueneHCID 11430Potassium CarbonateHCID 866453334-Methylphenyl borate

生成物 1

HCID 10633568HCID 10633568、化合物

試薬・触媒・溶媒 2

HCID 178418397HCID 178418397、化合物触媒HCID 962Water溶媒

実験手順

Under argon atmosphere, a mixture of 7-(trifluoromethanesulfoxy)-1-tetralone (9.02 g), 4-methylphenyl borate (5.00 g), potassium carbonate (8.46 g), toluene (300 ml), ethanol (30 ml) and water (30 ml)was stirred at room temperature for 30 minutes, and to the mixture was added tetrakis(triphenylphosphine)palladium (1.06 g). The mixture was refluxed for 14 hours. The reaction mixture was cooled to room temperature. The organic layer was separated, dried with anhydrous sodium sulfate, and concentrated under reduced pressure. The residue was separated and purified with column chromatography (ethyl acetate/toluene=1/10) to give 7-(4-methylphenyl)-1-tetralone (5.23 g) as colorless crystals.

後処理

  1. temperatureThe mixture was refluxed for 14 hours
  2. temperatureThe reaction mixture was cooled to room temperature
  3. customThe organic layer was separated
  4. dry with materialdried with anhydrous sodium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was separated
  7. custompurified with column chromatography (ethyl acetate/toluene=1/10)

出典と根拠

ORDレコード
ord-3e530ad227f143419817b9c75063798f
出典データセット
uspto-grants-2001_01
特許番号
US06172061B2

反応ノート

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