5-溴-2-(溴甲基)苯甲腈是重要的有机合成中间体,在医药研发、材料化学等领域有应用,可用于构建复杂有机分子骨架。
医药; 材料化学
合成路线 1(1. 合成:156001-53-5)
产率:70%
合成条件:With N-Bromosuccinimide; dibenzoyl peroxide In tetrachloromethane at 80℃; for 8 h; Inert atmosphere
实验步骤:将4-溴-2-甲基苄腈(10.0g,51.01mmol),N135(9.99g,56.11mmol)和过氧化苯甲酰(0.62g,2.6mmol)在CCl 4(100mE)中的混合物在80℃下搅拌 在N2气氛下8小时。 过滤混合物,将滤液浓缩至干。 残留物通过硅胶柱色谱纯化(0- EtOAc /石油醚溶液),得到标题化合物(9.8g,产率70%),为浅黄色油状物。 1 H NMR(400MHz,CDCl 3)ö7.8(d,J = 2.0Hz,1H),7.72(dd,J = 8.4,2.0Hz,1H),7.43(d,J = 8.4Hz,1H),4.58( s,2H)。
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