N-bromobutanimide → HCID 9822596、化合物
反応式
[CH3:1][O:2][C:3]([C:5]1[C:9]([NH:10][S:11]([C:14]2[CH:19]=[CH:18][C:17]([O:20][CH3:21])=[CH:16][CH:15]=2)(=[O:13])=[O:12])=[CH:8][S:7][CH:6]=1)=[O:4].C1C(=O)N([Br:29])C(=O)C1>CCOCC>[CH3:1][O:2][C:3]([C:5]1[C:9]([NH:10][S:11]([C:14]2[CH:19]=[CH:18][C:17]([O:20][CH3:21])=[CH:16][CH:15]=2)(=[O:13])=[O:12])=[C:8]([Br:29])[S:7][CH:6]=1)=[O:4]参加物
4
実験手順
To a solution of the product of Example 2 in 5.0 mL of AcOH--CHCl3 (1:1) at room temperature was added 0.299 g (1.682 mmol) of N-bromosuccimide. The reaction was stirred for 18 h and then diluted with ether, washed with water and saturated sodium bicarbonate solution, dried over MgSO4, filtered and concentrated in vacuo. The tan solid residue was washed with ether-hexanes (1:1) to provide 0.504 g (81%) of the desired product as a tan solid. Electrospray Mass Spec: 406.1 (M+H)+
後処理
- washwashed with water and saturated sodium bicarbonate solution
- dry with materialdried over MgSO4
- filtrationfiltered
- concentrationconcentrated in vacuo
- washThe tan solid residue was washed with ether-hexanes (1:1)
出典と根拠
- ORDレコード
- ord-4973688f20ef48739304649393e49b57
- 出典データセット
- uspto-grants-1999_10
- 特許番号
- US05962481
反応ノート
読み込み中…