Iodoethane → 2-Bromo-4-ethoxy-1-(trifluoromethoxy)benzene

HRID 1094821ノート

反応式

HRID 1094821 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([OH:13])[CH:5]=[CH:6][C:7]=1[O:8][C:9]([F:12])([F:11])[F:10].[CH2:14](I)[CH3:15].C(=O)([O-])[O-].[K+].[K+]>CC(C)=O>[Br:1][C:2]1[CH:3]=[C:4]([O:13][CH2:14][CH3:15])[CH:5]=[CH:6][C:7]=1[O:8][C:9]([F:11])([F:12])[F:10]

参加物

5

反応物 3

HCID 6340IodoethaneHCID 11430Potassium CarbonateHCID 27571943-bromo-4-(trifluoromethoxy)phenol

生成物 1

HCID 575823322-Bromo-4-ethoxy-1-(trifluoromethoxy)benzene収率 125%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

To a solution of the 3-bromo-4-trifluoromethoxyphenol (1.0 g, 2.48 mmol) in acetone (30 ml) was added ethyl iodide (0.795 ml, 9.94 mmol) followed by potassium carbonate (1.37 g, 9.94 mmol) and the reaction was heated to reflux for 12 hrs. The reaction mixture was cooled then filtered and concentrated in vacuo. Dichloromethane (20 ml) and water (20 ml) were added and the solution was filtered through a phase separation cartridge. The organic layer was collected, and evaporated in vacuo to afford crude title compound as a colourless oil (884 mg, 80%). Material was taken on without further purification.

後処理

  1. temperaturethe reaction was heated
  2. temperatureto reflux for 12 hrs
  3. temperatureThe reaction mixture was cooled
  4. filtrationthen filtered
  5. concentrationconcentrated in vacuo
  6. additionDichloromethane (20 ml) and water (20 ml) were added
  7. filtrationthe solution was filtered through a phase separation cartridge
  8. customThe organic layer was collected
  9. customevaporated in vacuo

出典と根拠

ORDレコード
ord-20340259bcdd4fb399ce84fc14ed2e5a
出典データセット
uspto-grants-2012_03
特許番号
US08134007B2

反応ノート

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