作为有机合成中间体,用于制备特定功能材料(如有机半导体、光电材料等),在材料化学研究中具有重要应用。
材料化学领域(如有机电子材料、光电材料等)
合成路线 1(1. 合成:91371-12-9)
产率:91%
合成条件:With copper In N,N-dimethyl-formamide at 125℃; for 1 h; Inert atmosphere
实验步骤:(1)在氮气氛下,将化合物No(1)(14.1g,50mmol)和铜粉(7.0g,109mmo -1)溶解在55mL N,N-二甲基甲酰胺中,在125℃搅拌该混合物。 °C 1小时然后停止。 冷却后,过滤残余物,用适量甲苯洗涤残余物,确保产物溶解在滤液中,滤液真空蒸馏,得到粗产物。 通过硅胶柱色谱法分离产物,并使用石油醚和二氯甲烷(v / v,4/1)作为洗脱剂在真空中分离,得到黄色固体,收率为91%,并进行1H NMR表征,证实黄色固体为 化合物号(2)
参考文献:
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合成路线 2(2. 合成:91371-12-9)
产率:84%
合成条件:With FeCl 3 In 1-methyl-pyrrolidin-2-one; hydrogenchloride
实验步骤:3,7-二氰基二苯并噻吩(14)。 将3,7-二溴二苯并噻吩(13,1.56g,4.56mmol)和氰化铜(I)(1.27g,14.2mmol)在1-甲基-2-吡咯烷酮(10mL)中的回流溶液在氮气下搅拌3小时。。 将冷却的反应混合物用FeCl 3(3.29g)的浓盐酸溶液处理。 HCl(10mL)。 在初始放热后,将混合物加热搅拌1小时。 将混合物倒在冰上。 将得到的灰色沉淀物滤出,干燥并升华(280℃,0.3mm Hg),得到白色粉末(0.89g,84%):mp> 330℃。 1H NMR(400MHz,DMSO-d6)δ8.76(s,2H),8.71(d,J = 8.2Hz,2H),8.01(dd,J = 8.2和1.4Hz,2H); HPLC(方法B)t R 16.84分钟(93.5面积%)。。 (C14H6N2S·0.25H2O)C,H,N。
参考文献:
- [1] Patent: US6172104, 2001, B2