反応式
[CH3:1][O:2][C:3]1[C:8]([CH2:9][N:10]2[CH2:15][CH2:14][CH:13]([CH2:16][OH:17])[CH2:12][CH2:11]2)=[CH:7][CH:6]=[CH:5][N:4]=1.C(N(CC)CC)C.O>CS(C)=O>[CH3:1][O:2][C:3]1[C:8]([CH2:9][N:10]2[CH2:11][CH2:12][CH:13]([CH:16]=[O:17])[CH2:14][CH2:15]2)=[CH:7][CH:6]=[CH:5][N:4]=1参加物
5
実験手順
16.1 g of 1-[(2-methoxy-3-pyridyl)methyl]-4-piperidinemethanol and 38 ml of triethylamine were suspended in 60 ml of dimethyl sulfoxide, a mixed solution of 21.7 g of a sulfur trioxide-pyridine complex and 100 ml of dimethyl sulfoxide was added dropwise thereto, and the mixture was stirred at room temperature for one hour. Water was added to the reaction solution, and the mixture was extracted with ethyl acetate. The organic layer was washed with brine, and then dried over anhydrous magnesium sulfate. The solvent was evaporated, and the crude product was purified by silica gel column chromatography (ethyl acetate), to give 10.9 g of the title compound 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
- customThe solvent was evaporated
- customthe crude product was purified by silica gel column chromatography (ethyl acetate)
出典と根拠
- ORDレコード
- ord-0338fe04f06843398eb7c5ed8d4d9ea5
- 出典データセット
- uspto-grants-2004_08
- 特許番号
- US06784192B2
関連ノート
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