反応式
[O:1]1[CH2:6][CH2:5][CH:4]([CH2:7][CH2:8][OH:9])[CH2:3][CH2:2]1.C(N(CC)CC)C.[CH3:17][S:18](Cl)(=[O:20])=[O:19]>ClCCl>[CH3:17][S:18]([O:9][CH2:8][CH2:7][CH:4]1[CH2:5][CH2:6][O:1][CH2:2][CH2:3]1)(=[O:20])=[O:19]参加物
5
実験手順
To a stirring solution of 2-(4-oxanyl)ethanol (9.63 g, 74.0 mmol) in dry dichloromethane (350 mL) was added distilled triethylamine (20.62 mL, 96.2 mmol) at 0° C., followed by drop-wise addition of methanesulfonyl chloride (7.44 mL, 96.2 mmol) over 15 min. The reaction was stirred for 16 h under N2 and slowly allowed to come to ambient temperature. The reaction was washed with saturated NaHCO3 (100 mL) and the aqueous phase was extracted with dichloromethane (1×50 mL). The combined organic extracts were dried (K2CO3), filtered and concentrated by rotary evaporation to yield 11.9 g of a colorless oil (77.0% yield).
後処理
- customto come to ambient temperature
- washThe reaction was washed with saturated NaHCO3 (100 mL)
- extractionthe aqueous phase was extracted with dichloromethane (1×50 mL)
- dry with materialThe combined organic extracts were dried (K2CO3)
- filtrationfiltered
- concentrationconcentrated by rotary evaporation
出典と根拠
- ORDレコード
- ord-b2772805d058453d89e0f64d57eedb50
- 出典データセット
- uspto-grants-2007_05
- 特許番号
- US07214686B2
関連ノート
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