Acetic Acid → Ethyl 3-bromo-6-hydroxy-2-methylbenzoate
反応式
[Br:1]Br.C(O)(=O)C.[CH3:7][C:8]1[C:13]([C:14]([O:16][CH2:17][CH3:18])=[O:15])=[C:12]([OH:19])[CH:11]=[CH:10][CH:9]=1>O.C(OCC)(=O)C>[Br:1][C:9]1[CH:10]=[CH:11][C:12]([OH:19])=[C:13]([C:8]=1[CH3:7])[C:14]([O:16][CH2:17][CH3:18])=[O:15]参加物
6
実験手順
A mixture of bromine (5.05 ml, 0.099 mol) and acetic acid (15 ml) is added to a mixture of ethyl 6-methyl-2-hydroxybenzoate (17.05 g, 0.095 mol), and acetic acid (15 ml) at a temperature of 20° C. The reaction mixture is stirred at room temperature for 1 hour. The reaction mixture is diluted with water and ethyl acetate. The organic phase is washed with water twice, concentrated in vacuo and the residue is purified by flash chromatography (petrol ethers:ethyl acetate, 98:2 v/v) yielding the pure product as a yellow oil, 21.7 g, (88.2%).
後処理
- washThe organic phase is washed with water twice
- concentrationconcentrated in vacuo
- customthe residue is purified by flash chromatography (petrol ethers:ethyl acetate, 98:2 v/v)
出典と根拠
- ORDレコード
- ord-a7b02d0bff1d45a7a3200b6dadfc077f
- 出典データセット
- uspto-grants-2000_10
- 特許番号
- US06127570
反応ノート
読み込み中…