偶氮二甲酸二异丙酯的合成

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2 h,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2 h,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。

Synthesis of Diisopropyl Azodicarboxylate

Isopropyl chloroformate and hydrazine were used as starting materials to prepare diisopropyl hydrazine-1,2-dicarboxylate, and then diisopropyl azodicarboxylate(DIAD) was prepared by oxidization with hydrogen peroxide. Factors influencing the reaction were investigated. Diisopropyl hydrazine-1,2-dicarboxylate was prepared by the reaction of hydrazine and chloroformate below 0 ℃ for 2 h in ether; under optimal reaction condition of n(diisopropyl hydrazine-1,2-dicarboxylate):n(hydrogen peroxide) with 1:1.1 at -5~5 ℃ for 2 h, the total yield of DIAD reached 90.7%. The structures of intermediate and product were characterized by IR and ¹H NMR.