摘要
以丙二腈为起始原料,采用一锅法在水相中反应制备了3-氨基-4-氨基肟基呋咱(AAOF)。通过考察亚硝化反应温度和闭环缩合的反应时间对目标产物收率的影响,确定了最佳反应条件为:亚硝化反应温度在30℃以下,闭环反应的回流时间为3 h。在该条件下,合成了5 kg级AAOF,其收率由以往的72.4%提高至85%以上,所得产物无需进一步重结晶提纯,且纯度大于99%。并用熔点、核磁、质谱和元素分析对产物的结构进行了表征。
3-Amino-4-aminoximinofurazan（AAOF） was synthesized from dicyanopropane by one-pot method in aqueous phase.The effects of the nitrosation reaction temperature and reaction time of ring closure and condensation on the yield of target product were observed;thereby the optimum conditions were determined as follows： the temperature of nistrosation reaction was lower than 30℃;the reflux time of ring closure reaction was 3 h.Under this condition,5 kg AAOF was synthesized.The yield was over 85%（72.4% traditionally）.With a high purity（99%）,the product needs no further purification by re-crystallization.Finally,the structure of AAOF was characterized by melting point,Mass,1HNMR and elemental analysis.
出处
《辽东学院学报（自然科学版）》
CAS
2010年第4期281-283,共3页
Journal of Eastern Liaoning University:Natural Science Edition
基金
"十五"国家科技攻关计划(2004BA304B)
