Water → 3,3-Dimethylbutyl methanesulfonate
反応式
[CH3:1][C:2]([CH3:7])([CH3:6])[CH2:3][CH2:4][OH:5].C(N(CC)CC)C.[CH3:15][S:16](Cl)(=[O:18])=[O:17].O>C1COCC1>[CH3:15][S:16]([O:5][CH2:4][CH2:3][C:2]([CH3:7])([CH3:6])[CH3:1])(=[O:18])=[O:17]参加物
6
実験手順
To a solution of 3,3-dimethylbutan-1-ol (20.2 g) and triethylamine (41.3 mL) in THF (200 mL) was added methanesulfonyl chloride (24.9 g) under ice-cooling, and the mixture was stirred for 1 hr. Water was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure and the residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (36.5 g) as a red-orange oil.
後処理
- temperaturecooling
- extractionthe mixture was extracted with ethyl acetate
- washThe extract was washed with saturated brine
- dry with materialdried over anhydrous magnesium sulfate
- customThe solvent was evaporated under reduced pressure
- customthe residue was purified by silica gel column chromatography (ethyl acetate/hexane)
出典と根拠
- ORDレコード
- ord-09a3ec4136bb499badd3916476705502
- 出典データセット
- uspto-grants-2016_07
- 特許番号
- US09382188B2
反応ノート
読み込み中…