Aluminium lithium hydride → HCID 9860329、化合物
反応式
C[O:2][C:3]([C@H:5]1[C@@H:10]([C:11]2[CH:16]=[CH:15][C:14]([Cl:17])=[C:13]([Cl:18])[CH:12]=2)[CH2:9][CH2:8][N:7]([CH3:19])[CH2:6]1)=O.[H-].[H-].[H-].[H-].[Li+].[Al+3]>O1CCCC1>[CH3:19][N:7]1[CH2:8][CH2:9][C@H:10]([C:11]2[CH:16]=[CH:15][C:14]([Cl:17])=[C:13]([Cl:18])[CH:12]=2)[C@H:5]([CH2:3][OH:2])[CH2:6]1参加物
4
反応条件
- 温度
- -30 °C
実験手順
A solution of (1) (5.0 g, 17 mmol) in tetrahydrofuran (50 ml) at −50° C. was added LiAlH4 (0.50 g, 13 mmol). Stirred at −30° C. for three hours, then quenched by addition of water and evaporated to a solid. The residue was dissolved in dichloromethane, dried with magnesium sulfate and evaporated to dryness. Yield 4.6 g of (3) (100%). Mp. 127-129° C.
後処理
- customquenched by addition of water
- customevaporated to a solid
- dissolutionThe residue was dissolved in dichloromethane
- dry with materialdried with magnesium sulfate
- customevaporated to dryness
出典と根拠
- ORDレコード
- ord-f6e2cd16ba6f44729086ded32bdbd24e
- 出典データセット
- uspto-grants-2009_07
- 特許番号
- US07560562B2
反応ノート
読み込み中…