偶氮二甲酸二异丙酯的合成

Synthesis of Diisopropyl Azodicarboxylate

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。

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.