反応式
[CH2:1]([N:8]1[CH2:12][CH2:11][C@@H:10](O)[CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.S(C1C=CC(C)=CC=1)([O-])(=O)=O.[F-:25].C([N+](CCCC)(CCCC)CCCC)CCC.O>C1COCC1>[CH2:1]([N:8]1[CH2:12][CH2:11][C@H:10]([F:25])[CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1参加物
5
実験手順
To a solution of (R)-1-benzyl-3-pyrrolidinol-tosylate (3.06 g, 9.24 mmol) in THF (30 ml) was added 1.0M solution of tetrabutylammonium fluoride in THF (37.0 ml 37.0 mmol) at room temperature. After 1.5 h stirring at reflux temperature, water (150 ml) was added to the reaction mixture and the mixture was extracted with ethyl acetate (100mix2). The combined extract was washed with water, brine, dried (Na2SO4), and concentrated to give brown oil, which was purified by column chromatography (silica gel: 80 g, CH2Cl2/MeOH 50/1) to afford 1.18 g (71%) of brown oil.
後処理
- additionwas added to the reaction mixture
- extractionthe mixture was extracted with ethyl acetate (100mix2)
- extractionThe combined extract
- washwas washed with water, brine
- dry with materialdried (Na2SO4)
- concentrationconcentrated
- customto give brown oil, which
- customwas purified by column chromatography (silica gel: 80 g, CH2Cl2/MeOH 50/1)
出典と根拠
- ORDレコード
- ord-ea4de7219b4046fd92e2d8cd81bd5517
- 出典データセット
- uspto-grants-2001_11
- 特許番号
- US06313302B2
関連ノート
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