3-(Methylthio)-1-propanol → 3-(Methylsulfanyl)propyl methanesulfonate
反応式
[CH3:1][S:2][CH2:3][CH2:4][CH2:5][OH:6].CCN(C(C)C)C(C)C.[CH3:16][S:17](Cl)(=[O:19])=[O:18]>ClCCl>[CH3:16][S:17]([O:6][CH2:5][CH2:4][CH2:3][S:2][CH3:1])(=[O:19])=[O:18]参加物
5
反応条件
- 温度
- -78 °C
実験手順
To a solution of 3-(methylthio)propan-1-ol in dichloromethane (0.2 M) was added sequentially at −78° C. Hunig's base (1.3 eq.) and methanesulfonyl chloride (1.3 eq.). The resulting reaction mixture was stirred at −78° C. for 1 h and then warmed slowly to RT. The reaction was quenched with sat. aq. NH4Cl and then extracted with ether. The combined organic extracts were washed with water and brine, dried over MgSO4, and filtered. Concentrated of the filtrate in vacuo afforded the title compound as a yellow oil.
後処理
- customThe resulting reaction mixture
- temperaturewarmed slowly to RT
- customThe reaction was quenched with sat. aq. NH4Cl
- extractionextracted with ether
- washThe combined organic extracts were washed with water and brine
- dry with materialdried over MgSO4
- filtrationfiltered
- concentrationConcentrated of the filtrate in vacuo
出典と根拠
- ORDレコード
- ord-deb24d9f41844cfbaf0712a398b6063c
- 出典データセット
- uspto-grants-2011_11
- 特許番号
- US08063105B2
反応ノート
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