Water → 2-(2,2-Difluorocyclopropyl)ethyl methanesulfonate
反応式
[CH3:1][S:2](Cl)(=[O:4])=[O:3].[F:6][C:7]1([F:13])[CH2:9][CH:8]1[CH2:10][CH2:11][OH:12].C(N(CC)CC)C.O>C1COCC1>[CH3:1][S:2]([O:12][CH2:11][CH2:10][CH:8]1[CH2:9][C:7]1([F:13])[F:6])(=[O:4])=[O:3]参加物
6
実験手順
Methanesulfonyl chloride (1.35 mL) was added to a solution of 2-(2,2-difluorocyclopropyl)ethanol (1.42 g) and triethylamine (3.24 mL) in THF (20 mL) dropwise at 0° C. The mixture was stirred at room temperature overnight. Water was added, and the mixture was extracted with ethyl acetate. The organic layer was washed with brine, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (hexane/ethyl acetate) to give the title compound (1.31 g) as a pale yellow oil.
後処理
- extractionthe mixture was extracted with ethyl acetate
- washThe organic layer was washed with brine
- dry with materialdried over anhydrous magnesium sulfate
- concentrationconcentrated under reduced pressure
- customThe residue was purified by silica gel column chromatography (hexane/ethyl acetate)
出典と根拠
- ORDレコード
- ord-ce7c07a2af9e4a64af00e512e8907a14
- 出典データセット
- uspto-grants-2014_05
- 特許番号
- US08729102B2
反応ノート
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