2,3,4,5,6,7-Hexahydro-1H-1-benzazonine-2,7-dione → 7-Hydroxy-1,3,4,5,6,7-hexahydro-2H-1-benzazonin-2-one
反応式
[NH:1]1[C:9]2[CH:10]=[CH:11][CH:12]=[CH:13][C:8]=2[C:7](=[O:14])[CH2:6][CH2:5][CH2:4][CH2:3][C:2]1=[O:15].[BH4-].[Na+]>C(O)C>[OH:14][CH:7]1[C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=2[NH:1][C:2](=[O:15])[CH2:3][CH2:4][CH2:5][CH2:6]1参加物
4
実験手順
A solution of 3,4,5,6-tetrahydro-1H-1-benzazonin-2,7-dione (14.2 g), J. Am. Chem. Soc. 88, 1049 (1966), and sodium borohydride (1.4 g) in ethanol (720 ml) is stirred at room temperature for 18 hours. The ethanol is removed under reduced pressure, and the residue dissolved in dichloromethane (350 ml). The solution is extracted with 2N hydrochloric acid (2×200 ml) and saturated brine (100 ml), and dried over sodium sulfate. The solvent is removed under reduced pressure to give 7-hydroxy-1,3,4,5,6,7-hexahydro-1-benzazonin-2-one.
後処理
- customThe ethanol is removed under reduced pressure
- dissolutionthe residue dissolved in dichloromethane (350 ml)
- extractionThe solution is extracted with 2N hydrochloric acid (2×200 ml) and saturated brine (100 ml)
- dry with materialdried over sodium sulfate
- customThe solvent is removed under reduced pressure
出典と根拠
- ORDレコード
- ord-0b72ee6ecc1545848586c964a8d265b2
- 出典データセット
- uspto-grants-1985_08
- 特許番号
- US04537885
反応ノート
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