Phosphorus tribromide → 1-(3-Bromopropyl)-4-methoxybenzene
反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([CH2:9][CH2:10][CH2:11]O)=[CH:5][CH:4]=1.P(Br)(Br)[Br:14]>>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([CH2:9][CH2:10][CH2:11][Br:14])=[CH:5][CH:4]=1参加物
3
実験手順
To a solution of 3-(p-methoxyphenyl)-1-propanol (16.6 g; 0.1 mol) in 250 mL of tolune, cooled to 0° C., was added dropwise 26 mL of phosphorus tribromide (0.27 mol). Following completion of the addition the reaction was stirred at room temperature for 1 hour, then refluxed for an additional hour. The reaction was cooled and poured onto ice, the layers were separated, and the organic phase washed with saturated sodium bicarbonate (3×) and brine (3×). The crude material obtained upon drying and evaporation of the solvent was chromatographed, eluting with 10%, EtOAc/hexane, to obtain 14 g (61%) of 3-(p-methoxyphenyl)-1-propylbromide.
後処理
- additioncompletion of the addition the reaction
- temperaturerefluxed for an additional hour
- temperatureThe reaction was cooled
- additionpoured onto ice
- customthe layers were separated
- washthe organic phase washed with saturated sodium bicarbonate (3×) and brine (3×)
- customThe crude material obtained
- customupon drying
- customevaporation of the solvent
- customwas chromatographed
- washeluting with 10%, EtOAc/hexane
出典と根拠
- ORDレコード
- ord-27845d3556614a0a81e759015d137572
- 出典データセット
- uspto-grants-1999_02
- 特許番号
- US05874449
反応ノート
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