Hydrochloric Acid → 1-[1-(Hydroxymethyl)cyclobutyl]ethanol
反応式
[Si]([O:8][CH2:9][C:10]1([CH:14]([OH:16])[CH3:15])[CH2:13][CH2:12][CH2:11]1)(C(C)(C)C)(C)C.[F-].C([N+](CCCC)(CCCC)CCCC)CCC.Cl>O1CCCC1>[OH:8][CH2:9][C:10]1([CH:14]([OH:16])[CH3:15])[CH2:13][CH2:12][CH2:11]1参加物
5
実験手順
1-[1-({[tert-Butyl(dimethyl)silyl]oxy}methyl)cyclobutyl]ethanol (3.2 g) was dissolved in tetrahydrofuran (30 mL), tetrabutylammonium fluoride (32 mL, 1.0 M tetrahydrofuran solution) was added dropwise, and the mixture was stirred at room temperature for 5 hr. The reaction mixture was added to 1 M hydrochloric acid, and the mixture was extracted with ethyl acetate/2-propanol (3/1). The organic layer was dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography to give the title compound as an oily compound (1.3 g, 79%).
後処理
- extractionthe mixture was extracted with ethyl acetate/2-propanol (3/1)
- dry with materialThe organic layer was dried over anhydrous magnesium sulfate
- customthe solvent was evaporated under reduced pressure
- customThe residue was purified by silica gel column chromatography
出典と根拠
- ORDレコード
- ord-7b0d63aad03442928c597879122b0b83
- 出典データセット
- uspto-grants-2014_12
- 特許番号
- US08921379B2
反応ノート
読み込み中…