Pyridine → HCID 19045537, 화합물
반응식
[CH2:1]([OH:9])[CH2:2][CH2:3][CH2:4][CH2:5][CH:6]([OH:8])[CH3:7].N1C=CC=CC=1.[CH3:16][S:17](Cl)(=[O:19])=[O:18]>ClCCl>[CH3:16][S:17]([O:9][CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH:6]([OH:8])[CH3:7])(=[O:19])=[O:18]참가 물질
5
실험 절차
(±)-Heptan-1,6-diol (1.06 g, 8 mmol) and pyridine (1.36 ml, 1.33 g, 16.8 mmol) were dissolved in dichloromethane (20 ml) and the mixture was cooled in ice. Methanesulfonyl chloride (0.65 ml, 0.96 g, 8.4 mmol) was added dropwise and the mixture was stirred at room temperature for 18 hours. Dichloromethane (50 ml) was added and the mixture was washed with aqueous HCl (1M, 50 ml) and brine (30 ml), dried (Na2SO4) and evaporated under reduced pressure. The residue was purified by flash column chromatography on silica gel, eluting with EtOAc/20% hexane, to give the alcohol as an oil (1.01 g, 60%).
후처리
- temperaturethe mixture was cooled in ice
- washthe mixture was washed with aqueous HCl (1M, 50 ml) and brine (30 ml)
- dry with materialdried (Na2SO4)
- customevaporated under reduced pressure
- customThe residue was purified by flash column chromatography on silica gel
- washeluting with EtOAc/20% hexane
출처 및 근거
- ORD 기록
- ord-d51ce0113ae04fb5a7097b9ef3ced9e7
- 출처 데이터셋
- uspto-grants-1993_04
- 특허 번호
- US05206240
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