Water → HCID 59267876、化合物
反応式
[Br:1]Br.[OH:3][CH2:4][C:5]([CH3:10])([CH3:9])[C:6](=[O:8])[CH3:7].C(OCC)(=O)C.O>CO>[Br:1][CH2:7][C:6](=[O:8])[C:5]([CH3:10])([CH3:9])[CH2:4][OH:3]参加物
6
実験手順
Bromine (182.0 g, 1.1 mol) is slowly added at −10° C. to a solution of 4-hydroxy-3,3-dimethyl-butan-2-one (120.0 g, 1.0 mol) in 700.0 mL of MeOH. The solution is slowly warmed up to room temperature and the reaction mixture is stirred for 2 h. Ethyl acetate and water are added to the reaction mixture, the two phases are separated, and the organic layer is washed with 10% K2CO3 solution. The organic layer is dried over anhydrous Na2SO4 and after filtration the solvent is removed under reduced pressure to afford the crude product that is purified by silica gel chromatography to afford 100.0 g of 1-bromo-4-hydroxy-3,3-dimethyl-butan-2-one as a brown liquid. Yield: 44%, over two steps; m/z 197 [M+H].
後処理
- customthe two phases are separated
- washthe organic layer is washed with 10% K2CO3 solution
- dry with materialThe organic layer is dried over anhydrous Na2SO4
- filtrationafter filtration the solvent
- customis removed under reduced pressure
- customto afford the crude product that
- customis purified by silica gel chromatography
出典と根拠
- ORDレコード
- ord-df23a58b227c4ebdaf2e32c447e4c538
- 出典データセット
- uspto-grants-2013_01
- 特許番号
- US08349871B2
反応ノート
読み込み中…