反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH3:9])=[CH:4][C:3]=1[C:10]1[CH:15]=[CH:14][C:13]([C:16]([O:18][CH3:19])=[O:17])=[CH:12][C:11]=1[C:20]1[C:24](=[O:25])[CH2:23][CH2:22][C:21]=1[CH3:26]>[Pd].CCOC(C)=O>[F:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH3:9])=[CH:4][C:3]=1[C:10]1[CH:15]=[CH:14][C:13]([C:16]([O:18][CH3:19])=[O:17])=[CH:12][C:11]=1[CH:20]1[C:24](=[O:25])[CH2:23][CH2:22][CH:21]1[CH3:26]参加物
4
実験手順
A pressure tube was charged with 66.56B (0.72 g, 2.0 mmol), EtOAc (20 mL), and Pd/C (10 wt. %) (0.22 g, 0.20 mmol). The tube was purged three times with H2 at 45 psi and sealed, and the contents were stirred for 48 hours. The mixture was filtered through silica gel (EtOAc) and concentrated. The crude product was purified by silica gel flash chromatography (0-20% EtOAc/hexane) to afford 66.56C (mixture of diastereomers) (0.63 g, 87% yield) as a colorless oil.
後処理
- customThe tube was purged three times with H2 at 45 psi
- customsealed
- filtrationThe mixture was filtered through silica gel (EtOAc)
- concentrationconcentrated
- customThe crude product was purified by silica gel flash chromatography (0-20% EtOAc/hexane)
出典と根拠
- ORDレコード
- ord-67ac87e675cf4f59b626f4fa626bf202
- 出典データセット
- uspto-grants-2011_10
- 特許番号
- US08030354B2
関連ノート
読み込み中…