Calcium Carbonate → 2-Bromo-5-fluorobenzyl alcohol
反応式
[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]参加物
5
実験手順
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).
後処理
- 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
出典と根拠
- ORDレコード
- ord-1076bffe427846ac8eb8c24fef4f4f01
- 出典データセット
- uspto-grants-2005_02
- 特許番号
- US06852711B2
反応ノート
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