N-bromobutanimide → 1-(-4-bromo-1-methyl-1H-imidazol-2-yl)-2,2,2-trichloroethanone
反応式
[Cl:1][C:2]([Cl:12])([Cl:11])[C:3]([C:5]1[N:6]([CH3:10])[CH:7]=[CH:8][N:9]=1)=[O:4].C1C(=O)N([Br:20])C(=O)C1>C1COCC1>[Br:20][C:8]1[N:9]=[C:5]([C:3](=[O:4])[C:2]([Cl:1])([Cl:11])[Cl:12])[N:6]([CH3:10])[CH:7]=1参加物
4
反応条件
- 温度
- -10 °C
実験手順
To the solution of 2,2,2-trichloro-1-(1-methyl-1H-imidazol-2-yl)ethanone (1.5 g, 6.6 mmol) in 26 mL of anhydrous THF was added 2.35 g of NBS at −10° C. The resulting mixture was stirred at −10° C. for 2 h, then 25° C. for 16 h. The solution was evaporated and the residue was purified by silica gel column (DCM as eluent) to give 1-(-4-bromo-1-methyl-1H-imidazol-2-yl)-2,2,2-trichloroethanone (1.18 g, yield 58%). 1H NMR (300 MHz, CDCl3) δ 7.15 (s, 1H), 4.05 (s, 3H).
後処理
- wait25° C. for 16 h
- customThe solution was evaporated
- customthe residue was purified by silica gel column (DCM as eluent)
出典と根拠
- ORDレコード
- ord-16ce7b993ae54b7eb52f787a05496fd1
- 出典データセット
- uspto-grants-2014_05
- 特許番号
- US08729078B2
反応ノート
読み込み中…