3-(Methylthio)-1-propanol → 3-(Methylsulfanyl)propyl methanesulfonate
반응식
[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]참가 물질
5
반응 조건
- 온도
- -78 °C
실험 절차
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.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-deb24d9f41844cfbaf0712a398b6063c
- 출처 데이터셋
- uspto-grants-2011_11
- 특허 번호
- US08063105B2
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