Dichloromethane → 2-(Methylsulfonyl)ethyl methanesulfonate
反応式
[CH3:1][S:2]([CH2:5][CH2:6][OH:7])(=[O:4])=[O:3].ClCCl.[CH3:11][S:12](Cl)(=[O:14])=[O:13].C(N(CC)C(C)C)(C)C>O>[S:12]([O:7][CH2:6][CH2:5][S:2]([CH3:1])(=[O:4])=[O:3])(=[O:14])(=[O:13])[CH3:11]参加物
6
実験手順
Combine 2-methylsulfonylethanol (7.7 g, 62 mmol) and dichloromethane (50 mL). Cool in an ice bath. Add methanesulfonyl chloride (7.81 g , 68.2 mmol). Add N,N-diisopropylethylamine (8.0 g, 62 mmol). After the addition of N,N-diisopropylethylamine, warm to ambient temperature. After 12 hours, add water and separate the layers. Extract the organic layer and extract with a saturated aqueous sodium bicarbonate solution. Dry the organic layer over Na2SO4, filter and evaporate in vacuo to give the title compound: mp; 55-57° C.
後処理
- temperatureCool in an ice bath
- customseparate the layers
- extractionExtract the organic layer
- extractionextract with a saturated aqueous sodium bicarbonate solution
- dry with materialDry the organic layer over Na2SO4
- filtrationfilter
- customevaporate in vacuo
出典と根拠
- ORDレコード
- ord-603f9c4a10a942f38dff287e78c1a030
- 出典データセット
- uspto-grants-2001_02
- 特許番号
- US06194406B1
反応ノート
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