Ethylene Glycol → 2-(5-Bromo-2-methylphenyl)-1,3-dioxolane
반응식
[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]=1참가 물질
5
반응 조건
- 온도
- 130 °C
실험 절차
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.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-5a0c0b5fb72943c9816dc6ef20695081
- 출처 데이터셋
- uspto-grants-2014_07
- 특허 번호
- US08791100B2
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