Ethyl Acetate → 2-Bromo-1-((2-(trimethylsilyl)ethoxy)methyl)-1H-imidazole
反応式
[CH3:1][Si:2]([CH3:13])([CH3:12])[CH2:3][CH2:4][O:5][CH2:6][N:7]1[CH:11]=[CH:10][N:9]=[CH:8]1.N#C[Br:16].CCOC(C)=O>C(#N)C>[Br:16][C:8]1[N:7]([CH2:6][O:5][CH2:4][CH2:3][Si:2]([CH3:13])([CH3:12])[CH3:1])[CH:11]=[CH:10][N:9]=1参加物
5
実験手順
To a solution of 107 (100 mg, 0.50 mmol) in acetonitrile (1 mL) at room temperature was added cyanogen bromide (107 mg, 1.0 mmol) and the mixture was allowed to stir at room temperature for 3 h, concentrated to dryness and partitioned between EtOAc and water. The organic phase was collected, dried over anhydrous sodium sulfate and concentrated to dryness. The residue was purified by column chromatography (eluents EtOAc/hexane 25:75, then EtOAc), to afford the title compound 108 (45 mg, 32% yield) as a colorless oil. MS (m/z) 277.0/279.0 (M+H).
後処理
- concentrationconcentrated to dryness
- custompartitioned between EtOAc and water
- customThe organic phase was collected
- dry with materialdried over anhydrous sodium sulfate
- concentrationconcentrated to dryness
- customThe residue was purified by column chromatography (eluents EtOAc/hexane 25:75
出典と根拠
- ORDレコード
- ord-645191db71334b60b77f31bf9d24e894
- 出典データセット
- uspto-grants-2010_08
- 特許番号
- US07772247B2
反応ノート
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