3-Hydroxy-3-methyl-2-butanone → 1,1-Dibromo-3-hydroxy-3-methylbutan-2-one
反応式
[CH3:1][C:2]([OH:7])([CH3:6])[C:3](=[O:5])[CH3:4].[Br-:8].[Br-:9].[Br-].[NH+]1C=CC=CC=1.[NH+]1C=CC=CC=1.[NH+]1C=CC=CC=1>ClCCl>[Br:8][CH:4]([Br:9])[C:3](=[O:5])[C:2]([OH:7])([CH3:6])[CH3:1]参加物
4
実験手順
To a stirred solution of 3-methyl-3-hydroxy-2-butanone (40 g, 0.392 mol) in anhydrous dichloromethane (2.2 l) under nitrogen was added solid pyridinium tribromide (250.4 g, 0.784 mol) in portions and the mixture was stirred at room temperature for 14 h. The mixture was then washed with dilute aqueous sodium hydrogensulphite (500 ml), then saturated aqueous NaCl (500 ml), dried (Na2SO4), and evaporated in vacuo. The residue was purified by flash chromatography (silica gel, CH2Cl2) to afford 31.4 g (31%) of the title compound as a colourless oil: 1H NMR (360 MHz, CDCl3) δ 1.54 (6H, s), 2.45 (1H, br s), 6.62 (1H, s).
後処理
- washThe mixture was then washed with dilute aqueous sodium hydrogensulphite (500 ml)
- dry with materialsaturated aqueous NaCl (500 ml), dried (Na2SO4)
- customevaporated in vacuo
- customThe residue was purified by flash chromatography (silica gel, CH2Cl2)
出典と根拠
- ORDレコード
- ord-3057822dd07c4c38a4c6d2f7a79b73dc
- 出典データセット
- uspto-grants-2007_02
- 特許番号
- US07176203B2
反応ノート
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