新型N-氨基取代的1,6-亚甲基桥[10]轮烯-3,4-二甲酰亚胺的无溶剂合成

Solvent-free Synthesis of Novel N-amino-substituted 1,6-Methanoannulene-3,4-dicarboximide

以1,6-亚甲基桥[10]轮烯-3,4-二乙酯为原料,简便地合成了二甲酸酐(2);2与肼在氮气保护下,无溶剂于170℃反应30 min,以较高收率合成了4个新型N-氨基取代的1,6-亚甲基桥[10]轮烯-3,4-二甲酰亚胺,其结构经1HNMR,13C NMR,MS及HR-MS表征。

1,6-Methano [ 10 ] annulene-3,4-dicarboxylic anhydride （2） was prepared from diethyl 1,6-methano [ 10 ] annulene-3,4-dicarboxylate, and then four novel N-amino substituted 1,6-methano [10]annulene-3,4-dicarboximides were synthesized in solvent-free by the reaction of 2 with hydrazines at 170 ℃ for 30 min under N2 atmosphere. The structures were characterized by 1H NMR, 13C NMR, MS and HR-MS.