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含能材料  2011 

高收率合成3-氨基-4-偕氨肟基呋咱研究

DOI: 10.3969/j.issn.1006-9941.2011.05.006

Keywords: 有机化学,3-氨基-4-偕氨肟基呋咱(AAOF),合成

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Abstract:

以丙二腈为原料,采用“两段法”合成了3-氨基-4-偕氨肟基呋咱(AAOF),利用红外光谱、核磁共振及元素分析等进行了结构表征;探讨了影响反应的关键因素,发现AAOF在碱性体系易生成钠盐是造成收率偏低的根本原因;优化了合成工艺条件,确定了适宜的反应条件为:亚硝化温度为5~10℃,肟化温度为25℃,脱水环化温度为105℃,体系pH值为7~8,总收率达95%,粗品纯度为98.5%。同时,采用差示扫描量热法(DSC)和热重/微商热重法(TG/DTG)研究了AAOF的热稳定性,其分解峰温为203.44℃。

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