以氯甲酸异丙酯、水合肼为主要原料,制备肼-1,2-二甲酸二异丙酯,然后用双氧水氧化制得偶氮二甲酸二异丙酯(DIAD).研究确定了最佳的反应条件:在0℃以下乙醚溶剂中,水合肼和氯甲酸异丙酯反应2h,制备肼-1,2-二甲酸二异丙酯;n(肼-1,2-二甲酸二异丙酯)∶n(双氧水)=1∶1.1,在-5 ～5℃下反应2h,双氧水氧化得到偶氮二甲酸二异丙酯,总收率为90.7％,采用红外光谱、核磁共振等技术手段验证了中间体及目标产物结构.
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