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作 者:范艳洁[1] 王伯周[1] 罗义芬[1] 周彦水[1] 杨润宁[1]
出 处:《化学试剂》2008年第10期739-742,共4页Chemical Reagents
基 金:国防973基础研究项目(613740102)
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.
关 键 词:有机化学 3-氨基-4-氰基呋咱 合成
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