摘要
以丙二腈为原料,一步法合成了3-氨基-4-酰氨肟基呋咱（AAOF）,然后用过氧化铅氧化得到了标题化合物,利用IR、^1HNMR、^13CNMR、元素分析进行结构表征,并确定最佳氧化反应条件：冰乙酸与AAOF的物质的量比为9∶1,过氧化铅与AAOF的物质的量比为1∶1,时间为1.5 h,温度为30-35℃,收率达到71.4%,高于文献报道（54%）;初步探索自行设计的CNAF分步合成路线,并从理论上分析3-氨基-2,3-二肟基丙腈未能脱水环化得到CNAF的原因。
3-Amino-4-aminoximidofurazan（AAOF） was synthesized by the one-step method using malononitrile as the starting material,followed by oxidization by lead dioxide（PbO2） to form CNAF.The molecular structure of CNAF was identified by IR,^1HNMR,^13CNMR and elemental analysis.The optimal condition for oxidization reaction was confirmed as follows：the ratio between acetic acid and AAOF was 9∶1,the ratio between PbO2 and AAOF was 1∶1,the reaction time was 1.5 h,and the reaction temperature was 30～35 ℃.Under these conditions,the yield of CNAF was 71.4%,which was much higher than the yield reported in the literature.A self-designed pathway for stepwise synthesis of CNAF was also explored,and the reason why CNAF cannot be synthesized from 3-amino-2,3-di（hydroxyimino）propionitrile was also analyzed theoretically.
出处
《化学试剂》
CAS
CSCD
北大核心
2008年第10期739-742,共4页
Chemical Reagents
基金
国防973基础研究项目(613740102)
作者简介
范艳洁（1983-），女，浙江慈溪人，硕士生，从事有机合成研究。
