Ethylene Glycol → 2-(5-Bromo-2-methylphenyl)-1,3-dioxolane
反応式
[Br:1][C:2]1[CH:3]=[CH:4][C:5]([CH3:10])=[C:6]([CH:9]=1)[CH:7]=[O:8].[CH2:11](O)[CH2:12][OH:13].O.C1(C)C=CC(S(O)(=O)=O)=CC=1>C1(C)C=CC=CC=1>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([CH3:10])=[C:6]([CH:7]2[O:13][CH2:12][CH2:11][O:8]2)[CH:9]=1参加物
5
反応条件
- 温度
- 130 °C
実験手順
To a solution of INT 30 (17.3 g, 87 mmol) in toluene (505 mL) was added ethane-1,2-diol (24.3 mL, 436 mmol) followed by p-toluenesulfonic acid monohydrate (0.83 g, 4.36 mmol). The reaction mixture was stirred at 130° C. for 21 hours. The mixture was washed with saturated aqueous NaHCO3 (2×) and brine (2×). The organic layer was dried over MgSO4, filtered and concentrated. The residue was purified by Kugelrohr distillation to give INT 31.
後処理
- washThe mixture was washed with saturated aqueous NaHCO3 (2×) and brine (2×)
- dry with materialThe organic layer was dried over MgSO4
- filtrationfiltered
- concentrationconcentrated
- distillationThe residue was purified by Kugelrohr distillation
- customto give INT 31
出典と根拠
- ORDレコード
- ord-5a0c0b5fb72943c9816dc6ef20695081
- 出典データセット
- uspto-grants-2014_07
- 特許番号
- US08791100B2
反応ノート
読み込み中…