反応式
[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]1参加物
4
反応条件
- 温度
- -10 °C
実験手順
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).
後処理
- 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
出典と根拠
- ORDレコード
- ord-f93bcc193765440ea9dd7eada4782451
- 出典データセット
- uspto-grants-2014_09
- 特許番号
- US08829052B2
関連ノート
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