5851-46-7 2-戊基苯并咪唑
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分子式C12H16N21.592溶解度0.0427 mg/ml ; 0.000227 mol/l 酸度系数(pKa)11.99±0.10 (Predicted) 8.5,过滤,水洗至中性,乙醇-水混合溶剂(体积比1:2
条件: Stage #1: at 110℃; for 3 h; Stage #2: at 140℃; for 1.50 h产率: 90%参考文献: [1] Synthetic Communications, 2007, vol.37, #15, p.2457-2460; [2] Patent: CN103483266, 2016, B. Location in patent: Paragraph 0041; 0042; 0043; 0044; [3] Annales Pharmaceutiques Francaises, 2003, vol.61, #1, p.57-61; [4] Synthetic Communications, 2002, vol.32, #24, p.3703-3709; [5] New Journal of Chemistry, 2007, vol.31, #8, p.1417-1420; [6] Journal of the Chemical Society, 1937, p.1699; [7] Monatshefte fuer Chemie, 1931, vol.57, p.97,104; [8] Journal of the American Chemical Society, 1937, vol.59, p.178合成路线 3(5851-46-7)
- 步骤: 向25mL圆底烧瓶中加入邻苯二胺(1)(0.108g,1mmol)、三丁胺(2a)(0.185g,1mmol)、5%Pd/C(0.106g,0.05mmol)和甲苯/H₂O(10mL/0.5mL)的混合物,Ar冲洗后在110℃反应20小时。反应混合物通过短硅胶柱(乙酸乙酯-己烷)过滤除催化剂,减压除去溶剂,薄层色谱(硅胶,乙酸乙酯-己烷=1/1)分离得产物。
- 条件: With 5%-palladium/activated carbon In water; toluene at 110℃; for 20 h; Inert atmosphere
- 产率: 57%
- 参考文献: [1] Bulletin of the Korean Chemical Society, 2012, vol.33, #12, p.4188-4190
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