作为有机合成中间体,用于制备功能性材料或药物分子,在材料化学领域有潜在应用。
有机合成; 材料化学
合成路线 1(1. 合成:136630-36-9)
产率:85%
合成条件:With hydrogenchloride; tin In ethanol; water at 70℃; for 1 h; Inert atmosphere
实验步骤:(2)在氮气氛下,将化合物2(4.02g,10mmol)溶于48mL乙醇和30mL水溶液中,在搅拌下缓慢加入锡粉(5.94g,50mmol),然后加热至80℃。 在70℃下保持1小时,停止加热,将反应烧瓶放入冰水浴中,逐渐加入2mol / L氢氧化钠水溶液直至反应体系变为碱性。 然后用二氯甲烷萃取,收集有机相并用无水硫酸钠干燥。 通过硅胶柱色谱法分离产物,并使用石油醚和四氢呋喃(v / v,20/1)作为洗脱剂在真空中分离,使用1 H NMR得到85%收率的浅灰色固体。 确认黄色固体为化合物3
参考文献:
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合成路线 2(2. 合成:136630-36-9)
产率:81%
合成条件:Stage #1: With copper In N,N-dimethyl-formamide for 3 h; Reflux Stage #2: With hydrogenchloride; tin In water; N,N-dimethyl-formamide for 6 h; Cooling with ice
实验步骤:将2,5-二溴硝基苯(4.5g,16mmol)溶于N'N-二甲基甲酰胺中,加入铜粉(0.2g,3mmol),将该反应物在回流下搅拌3小时,冷却后,加入锡粉 加入(0.2g,1.7mmol),冰盐浴条件加入10ml盐酸,搅拌6小时,真空干燥蒸发溶剂,然后将固体溶解在乙酸乙酯中,搅拌,过滤,用饱和盐水洗涤3次, 在真空汽蒸下将溶剂蒸发至干,通过硅胶柱色谱法纯化,得到固体化合物23a(4.65g,13mmol),收率81%。
参考文献:
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