反応式
[Br:1][C:2]1[CH:3]=[CH:4][C:5]([F:10])=[C:6]([CH2:8][OH:9])[CH:7]=1.[H-].[Na+].[CH3:13]I.O>C1COCC1>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([F:10])=[C:6]([CH2:8][O:9][CH3:13])[CH:7]=1参加物
6
実験手順
To a solution of (5-bromo-2-fluorophenyl)methanol (5.00 g) in THF (100 ml) was added 60% sodium hydride (1.08 g) at 0° C., and the mixture was stirred at room temperature for 30 min. Methyl iodide (3.80 ml) was added, and the mixture was stirred for 1.5 h. Water was added to the reaction mixture, and the mixture was extracted with ethyl acetate, washed with saturated brine and dried. The solvent was evaporated under reduced pressure and the residue was purified by column chomatography (eluent, hexane→hexane:ethyl acetate=50:1) to give the title compound (4.86 g) as a brown oil.
後処理
- stirringthe mixture was stirred for 1.5 h
- extractionthe mixture was extracted with ethyl acetate
- washwashed with saturated brine
- customdried
- customThe solvent was evaporated under reduced pressure
- customthe residue was purified by column chomatography (eluent, hexane→hexane:ethyl acetate=50:1)
出典と根拠
- ORDレコード
- ord-2d70ab7af45e46089630058db1ad1a66
- 出典データセット
- uspto-grants-2003_02
- 特許番号
- US06518257B1
関連ノート
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