1-[4-(4-氯苯基)-2-羟基正丁基]咪唑为杂环有机物,可用作医药中间体。
医药
合成路线 1(1. 合成:67085-11-4)
产率:99.31%
合成条件:With sodium hydride In N,N-dimethyl-formamide at 58 - 62℃; for 3 h; Cooling with ice
实验步骤:(2)在DMF中加入浓度为20%的氢化钠,在冰冷却下,以20ml浓度的咪唑在DMF中的搅拌速度滴加至2ml / s,在60℃下搅拌60min,在冰冷却后将盐浴法缓慢加入到中间产物1中,将DMF的氢化钠,咪唑在DMF中和中间产物的重量比为7:7:5,在60℃下在120min反应混合物中搅拌,在冰冷却后盐浴法,向反应混合物中加入25重量%正己烷的反应溶液,以3rev / sec的速度进行反应,搅拌15min后,加入反应溶液,考虑到冰的重量为350%,用3转/秒搅拌蒸馏沉淀过滤沉淀物过滤后,滤饼重量为过滤饼重量的1/3,用水洗涤一次,以速度2830r / min条件离心干燥60min用离心机将所得产物重量的2.5倍干燥,用乙酸乙酯和活性炭干燥0.05倍,在5℃下静置13小时,50℃重结晶,并通过重结晶得到的产物干燥。通过HPLC检测中间体2。中间体2 71.5%收率,其中所需产物1(2-羟基-4(4-氯苯基)丁酸Y1)1H-氢咪唑类化合物为99.31%
参考文献:
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