- 概述
4-碘-2,6-二甲基苯胺是一种有机中间体,可由2,6-二甲基苯胺碘代制备得到。4-碘-2,6-二甲基苯胺的氨基可以通过重氮化制备二甲基对溴碘代苯。
- 4-碘-2,6-二甲基苯胺是有机合成中间体和医药中间体,可用于实验室研发过程和化工医药合成过程中。
- 制备
将充分研磨的碘12.7g(0.05mol)、40mL乙酸乙酯和50mL乙酸加入250mL三颈烧瓶中,搅拌下分批加入SPC 7.5g(0.054mol),20min内加完。再加入2,6-二甲基苯胺12.4mL(0.1mol),20~25℃搅拌0.5h后,升温至45~50℃,回流1h。冷却后,将混合物倒入200mL w(Na2SO3)=5%的水溶液中,充分搅拌后,有机相减压蒸去溶剂得黑紫色固体粗产物,经正己烷重结晶得白色针状晶体4-碘-2,6-二甲基苯胺10.5g,收率42.5%。
有机合成; 医药
合成路线 1(1. 合成:4102-53-8)
产率:93%
合成条件:at 80℃; for 2 h;
实验步骤:通用方法:将芳族/杂芳族胺(1mmol)和二氯碘酸1-丁基-3-甲基吡啶鎓(BMPDCI)(1.2mmol)的混合物加热至80℃,保持1-4小时。 反应完成后(通过TLC监测),加入乙酸乙酯,然后加入水。 分离有机层,水层用乙酸乙酯萃取三次。 将合并的有机层用硫酸钠干燥并在真空下蒸发,得到粗产物,使用硅胶进一步进行柱色谱,得到如表1所示的纯碘化产物。
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