Pyridine → HCID 19045537、化合物
反応式
[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]参加物
5
実験手順
(±)-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%).
後処理
- 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
出典と根拠
- ORDレコード
- ord-d51ce0113ae04fb5a7097b9ef3ced9e7
- 出典データセット
- uspto-grants-1993_04
- 特許番号
- US05206240
反応ノート
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