Methyl iodide → 4-Bromo-2,6-difluoroanisole

HRID 746770

反応式

HRID 746770 の反応式
IC.[Br:3][C:4]1[CH:9]=[C:8]([F:10])[C:7]([OH:11])=[C:6]([F:12])[CH:5]=1.[C:13](=O)([O-])[O-].[K+].[K+].ClCCl>CC(C)=O>[Br:3][C:4]1[CH:9]=[C:8]([F:10])[C:7]([O:11][CH3:13])=[C:6]([F:12])[CH:5]=1

参加物

6

反応物 4

HCID 6328Methyl iodideHCID 6344DichloromethaneHCID 11430Potassium CarbonateHCID 27362924-Bromo-2,6-difluorophenol

生成物 1

HCID 27732874-Bromo-2,6-difluoroanisole

試薬・触媒・溶媒 1

HCID 180Acetone溶媒2 回

実験手順

Add iodomethane (2.0 ml, 32.1 mmol) dropwise to a suspension of 4-bromo-2,6-difluorophenol (5.90 g, 28.2 mmol) and potassium carbonate (4.40 g, 31.8 mmol) in acetone (50 ml) at room temperature while stirring vigorously. Heat the mixture under reflux overnight. Evaporate acetone and add dichloromethane. Filter through silica eluting the product with dichloromethane/EtOAc. Concentrate to yield the title compound.

後処理

  1. temperatureHeat the mixture
  2. temperatureunder reflux overnight
  3. filtrationFilter through silica eluting the product with dichloromethane/EtOAc
  4. concentrationConcentrate

出典と根拠

ORDレコード
ord-a291ed1aa0994e328206e6d5aeacc4dc
出典データセット
uspto-grants-2008_07
特許番号
US07393868B2

関連ノート

読み込み中…