반응 #595321
ord-46d4d42143234c33aaa63af1caee4cdb
반응 방정식
Cyclopropanesulfonyl chloride
BuOH
pyridine
→
oil
수율 71.0%
Butyl cyclopropanesulfonate
수율 71.0%
반응 조건
온도
-10°CELSIUS
상세 조건
See reaction.notes.procedure_details.
후처리
- 1온도The mixture was slowly warmed at room temperature
- 2기타The solvent was removed under reduced pressure
- 3workup.DISSOLUTIONthe resulting white solid was dissolved in CHCl3
- 4세척The organic phase was washed with water, brine
- 5건조dried (MgSO4)
- 6농축concentrated
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), 0.93 (t, 3H).