合成路线 1(1. 合成:7567-63-7)
产率:87%
合成条件:Stage #1: With caesium carbonate In methanol for 16 h; Stage #2: With ammonium chloride In dichloromethane; water
实验步骤:(9)1,3,5-三乙炔基苯。 在氩气下向火焰干燥的烧瓶中加入(8)(2.39mmol,1当量),碳酸铯(4.78mmol,2当量)和甲醇(10mL)。 将反应搅拌16小时。 完成后,解决方案从不透明变为半透明。 真空除去甲醇,将固体在水和二氯甲烷之间分配。 用二氯甲烷(3×20mL)萃取水层。 用氯化铵水溶液(1.0M,2×20mL),水(2×20mL)和盐水(2×20mL)洗涤有机层。 用硫酸钠干燥有机层,过滤,并真空除去。 得到产物,为灰白色软晶体(2.09mmol),产率87%,熔点101-103℃.1H NMR(400MHz,CDCl3)δ7.57(s,3H),3.12(s,3H)。 13 C NMR(100MHz,CDCl 3)δ135.6,122.8,81.6,78.7。 MS(CI +)m / z 151 [M] +。
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