化学合成。
有机合成; 医药化工
合成路线 1(1. 合成:63262-06-6)
产率:73%
合成条件:at 0 - 20℃; for 33 h;
实验步骤:向250ml反应烧瓶中加入2.66g(11.7mmol)高碘酸钾,降温至0℃,加入60ml浓硫酸。 搅拌,加入5.82g(35.1mmol)碘化钾,15分钟后,加入5.52g(23.4mmol)至两溴苯和24ml浓硫酸,0℃下反应18小时。 将温度逐渐升至室温,反应15小时。 将反应溶液倒入冰中的瓶中,搅拌,过滤得到的滤饼为1,4-二溴-2,5-二碘化物粗产物,溶解滤饼加,稀NaOH溶液洗涤,萃取, 有机相干燥,浓缩,重结晶,得8.326g(产率73%)1,4-二溴-2,5-二碘化物,用氯仿和四氢呋喃作为混合溶剂的溶剂重结晶,在氯仿中混合溶液:四氢呋喃= 2:1。
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