化学合成。
有机合成; 材料中间体
合成路线 1(1. 合成:56525-79-2)
产率:76%
合成条件:With tetrakis(triphenylphosphine) palladium (0) ; potassium carbonate In tetrahydrofuran; water at 80℃; for 16 h; Inert atmosphere
实验步骤:将其在氮气环境中在700mL四氢呋喃(THF)中溶于3,6-二溴-9H-咔唑(100g,308mmol),此处为苯基硼酸(45.1g,370mmol)并加入四(三苯基膦)钯。 搅拌(10.7g,9.24mmol)。 在饱和水中的碳酸钾(213g,1,540mmol)中,在80℃下加热回流16小时。 反应完成后,将反应溶液加入水中,用DCM萃取,然后用无水MgSO 4除去水,过滤,减压浓缩。 因此,将所得残余物通过快速柱色谱法分离和纯化,得到化合物I-23(74.8g,76%)。
参考文献:
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