3，3′-二（N-羟基偕胺肟基）二呋咱基醚合成及歧化反应

摘要

3,3′-Bis ( N-hydroxy amidoxime) difurazanyl ether was synthesized from 3-cyano-4-nitrofurazan via etherification of nitro-group, addition, diazotisation and dioximation reaction with a total yield of 51.0%, and its structure and intermediates were characterized by IR, NMR and elemental analysis.The reaction conditions of dioximation were discussed and the optimum condi-tion was obtained as follows:reaction temperature 20 ℃, n(DCFOF):n(NH2 OH・ HCl):n(KOH)=1:4:4.Under alkaline conditions, DOFOF could be easily disproportionated to obtain 3,3′-diamidoximinodifurazanyl ether.In addition, the reaction mechanism for disproportionation reaction of DOFOF was proposed.%以3-氰基-4-硝基呋咱为原料，经分子间醚化、加成、重氮化、双肟化得到3，3′-二（N-羟基偕胺肟基）二呋咱基醚（DOFOF），总收率达51．0％，用IR、1 H NMR、13 C NMR、元素分析等进行了结构表征。初步优化了双肟化工艺，确定了最佳反应条件：反应温度20℃，n（DCFOF）瞷n（NH2 OH・ HCl）瞷n（KOH）＝1瞷4瞷4。发现了 DOFOF 在碱性条件下易发生歧化反应，分离鉴定了歧化产物3，3′-二偕胺肟基二呋咱基醚，并从理论上提出了可能的歧化反应机理。