Sulfuric Acid → HCID 22261682、化合物
反応式
[OH:1][C:2]1[CH:3]=[C:4]([CH:10]=[CH:11][CH:12]=1)[C:5]([O:7][CH2:8][CH3:9])=[O:6].[CH2:13]=[C:14]([CH3:16])[CH3:15].S(=O)(=O)(O)O>ClCCl>[C:14]([O:1][C:2]1[CH:3]=[C:4]([CH:10]=[CH:11][CH:12]=1)[C:5]([O:7][CH2:8][CH3:9])=[O:6])([CH3:16])([CH3:15])[CH3:13]参加物
5
実験手順
To a solution of ethyl 3-hydroxybenzoate (20 g, 0.13 mol) in dichloromethane (200 ml) were added isobutene (about 30 g) and conc. sulfuric acid (0.5 ml), and the mixture was left for 2 days. The reaction solution was washed with saturated aqueous sodium hydrogen carbonate solution, dried over anhydrous magnesium sulfate and evaporated under reduced pressure. The residue was purified by silica gel chromatography (hexane:ethyl acetate=10:1) to give the objective substance (17.3 g, 63%) as an oil.
後処理
- washThe reaction solution was washed with saturated aqueous sodium hydrogen carbonate solution
- dry with materialdried over anhydrous magnesium sulfate
- customevaporated under reduced pressure
- customThe residue was purified by silica gel chromatography (hexane:ethyl acetate=10:1)
- customto give the objective substance (17.3 g, 63%) as an oil
出典と根拠
- ORDレコード
- ord-d44bede4e3ee4c1785b0220770d19feb
- 出典データセット
- uspto-grants-2006_01
- 特許番号
- US06982348B2
反応ノート
読み込み中…