化学合成。
化学合成
合成路线 1(1. 合成:3401-47-6)
产率:83%
合成条件:With potassium carbonate In N,N-dimethyl-formamide at 20℃; for 12 h; Inert atmosphere
实验步骤:将7.0g(345.2mmol)中间体M-1和95.4g(690.4mmol)碳酸钾加入到2000mL烧瓶中的1000mL N,N-二甲基甲酰胺中,然后加入32.2ml甲基碘(MeI)(517.7)。 缓慢滴加(mmol)。然后,在氮气流下将混合物在室温下搅拌12小时。将所得混合物加入到3000mL蒸馏水中,过滤结晶的固体,得到中间体M-2(101.1)。 g,83%产量)。
参考文献:
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合成路线 2(2. 合成:3401-47-6)
产率:98%
合成条件:With tris(2,2'-bipyridyl)ruthenium dichloride; carbon tetrabromide In acetonitrile at 20℃; Irradiation
实验步骤:一般步骤:向装有磁力搅拌棒的10mL圆底烧瓶中加入酚类或烯烃(0.1mmol),CBr4(33mg,0.1mmol),无水CH3CN(1mL)和Ru(bpy)3Cl2(3.8mg) ,0.005毫摩尔)。 在室温下将混合物用蓝色LED(1W)照射,通入空气直至原料完全消失(通过TLC监测)。 反应完成后,将溶剂真空浓缩。 通过快速柱色谱法纯化残余物,得到最终产物。
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