Calcium Carbonate → 2-Bromo-5-fluorobenzyl alcohol
반응식
[Br:1][C:2]1[CH:9]=[CH:8][C:7]([F:10])=[CH:6][C:3]=1[CH2:4]Br.C([O-])([O-])=[O:12].[Ca+2]>O1CCOCC1.O>[Br:1][C:2]1[CH:9]=[CH:8][C:7]([F:10])=[CH:6][C:3]=1[CH2:4][OH:12]참가 물질
5
실험 절차
2-Bromo-5-fluorobenzylbromide (2.0 g, 7.46 mmol) was dissolved in dioxane (25 mL) and H2O (25 mL), and CaCO3 (3.84 g, 38.39 mmol) was added. The mixture was heated to reflux overnight. The solution was concentrated, and the residue was partitioned between H2O and CH2Cl2. The organic phase was washed with 1N HCl and brine, dried (MgSO4), filtered, and concentrated to afford the title compound. 1H NMR (CDCl3): δ 2.00 (t, 1H), 4.72 (d, 2H), 6.85-6.92 (m, 1H), 7.26 (dd, 1H), 7.48 (dd, 1H).
후처리
- temperatureThe mixture was heated
- temperatureto reflux overnight
- concentrationThe solution was concentrated
- customthe residue was partitioned between H2O and CH2Cl2
- washThe organic phase was washed with 1N HCl and brine
- dry with materialdried (MgSO4)
- filtrationfiltered
- concentrationconcentrated
출처 및 근거
- ORD 기록
- ord-1076bffe427846ac8eb8c24fef4f4f01
- 출처 데이터셋
- uspto-grants-2005_02
- 특허 번호
- US06852711B2
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