90560-10-4 6-甲氧基苯并噻吩
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安全说明
危险性质:非危险化学品
用途与制备
化学合成。
化学合成
96803-85-9 90560-10-4 方法B:将粗制的1-(2,2-二乙氧基乙基硫烷基)-3-甲氧基苯(8.27 g,32.3 mmol)溶于己烷(100 mL)中,缓慢滴加到含有甲磺酸(1.05 mL,1.55 g,16.1 mmol)和硅藻土(16.5 g)的己烷(1000 mL)溶液中。将反应混合物加热回流1小时。反应完成后,冷却至室温,加入三乙胺(4.5 mL,3.26 g,32.3 mmol)以终止反应。过滤粗反应混合物,将滤液在减压下浓缩,得到红色油状物。通过硅胶柱色谱法对产物进行纯化,使用己烷/乙醚(98:2)作为洗脱剂。收集合适的馏分并蒸发溶剂,得到3.35 g(63%收率)的无色油状目标产物6-甲氧基苯并[b]噻吩。产物的1H NMR(DMSO-d6)数据如下:δ 7.74(1H,d,J = 8.7 Hz),7.56(1H,d,J = 2.3 Hz),7.52(1H,d,J = 5.3 Hz),7.33(1H,d,J = 5.3 Hz),6.99(1H,dd,J = 2.3, 8.7 Hz),3.81(3H,s)。元素分析计算值(C9H8OS):C,65.82;H,4.91;S,19.53。实测值:C,66.01;H,5.00;S,19.40。 参考文献: [1] Patent: WO2003/106462, 2003, A1. Location in patent: Page 34 [2] Patent: US2006/52378, 2006, A1. Location in patent: Page/Page column 149 [3] Patent: WO2003/106462, 2003, A1. Location in patent: Page 34 [4] Patent: WO2005/73206, 2005, A1. Location in patent: Page/Page column 23-27 [5] Patent: US2009/286863, 2009, A1. Location in patent: Page/Page column 7-8