Methanol → Methyl 2-bromo-2-(4-fluorophenyl)acetate
反応式
[Br:1][CH:2]([C:6]1[CH:11]=[CH:10][C:9]([F:12])=[CH:8][CH:7]=1)[C:3]([OH:5])=[O:4].[CH3:13]O>>[Br:1][CH:2]([C:6]1[CH:11]=[CH:10][C:9]([F:12])=[CH:8][CH:7]=1)[C:3]([O:5][CH3:13])=[O:4]参加物
3
実験手順
The α-bromo-4-fluorophenylacetic acid from Part 1 was dissolved in methanol (100 ml) and was added Dowex-50X-400® (2.7 g) to the solution. The mixture was refluxed for 6 hours and the resin was removed by filtering through Celite® after cooling. The filtrate was evaporated to give an oily residue, which was purified by column chromatography on silica gel with elution by 1:9 ethyl acetate-hexane to afford methyl α-bromo-4-fluorophenylacetate (87% yield).
後処理
- additionwas added Dowex-50X-400® (2.7 g) to the solution
- temperatureThe mixture was refluxed for 6 hours
- customthe resin was removed
- filtrationby filtering through Celite®
- temperatureafter cooling
- customThe filtrate was evaporated
- customto give an oily residue, which
- customwas purified by column chromatography on silica gel with elution by 1:9 ethyl acetate-hexane
出典と根拠
- ORDレコード
- ord-f1c151c8a57848b3b032dbab0a2ec812
- 出典データセット
- uspto-grants-1996_12
- 特許番号
- US05583147
反応ノート
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