반응식
[CH:1]1([S:4](Cl)(=[O:6])=[O:5])[CH2:3][CH2:2]1.N1C=CC=CC=1.[CH2:14]([OH:18])[CH2:15][CH2:16][CH3:17]>>[CH:1]1([S:4]([O:18][CH2:14][CH2:15][CH2:16][CH3:17])(=[O:6])=[O:5])[CH2:3][CH2:2]1참가 물질
4
반응 조건
- 온도
- -10 °C
실험 절차
Cyclopropanesulfonyl chloride (5 g, 35 mmol, 1 eq) was dissolved in an excess BuOH (20 ml), the reaction mixture was cooled at −10° C. and pyridine (5.8 mL, 70 mmol, 2 eq) was slowly added dropwise. The mixture was slowly warmed at room temperature and stirred overnight. The solvent was removed under reduced pressure and the resulting white solid was dissolved in CHCl3. The organic phase was washed with water, brine and dried (MgSO4) and concentrated to give an oil (4.8 g, 24.9 mmol, 71%). 1H NMR (300 MHz, CDCl3): δ 4.25 (t, 2H), 2.46 (m, 1H), 1.74 (m, 2H), 1.45 (m, 2H), 1.25 (dd, 2H), 1.09 (dd, 2H), 93 (t, 3H).
후처리
- temperatureThe mixture was slowly warmed at room temperature
- customThe solvent was removed under reduced pressure
- dissolutionthe resulting white solid was dissolved in CHCl3
- washThe organic phase was washed with water, brine
- dry with materialdried (MgSO4)
- concentrationconcentrated
출처 및 근거
- ORD 기록
- ord-f93bcc193765440ea9dd7eada4782451
- 출처 데이터셋
- uspto-grants-2014_09
- 특허 번호
- US08829052B2
연결된 노트
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