3,4-二(吡嗪-2′-基)氧化呋咱的合成与表征

Synthesis and Characterization of 3,4-Bis(pyrazine-2′yl)furoxan

以2-氰基吡嗪为原料，经肟化、重氮化、脱氮、环化四步反应合成出-3，4-二（吡嗪2’-基）氧化呋咱（DPF），总收率为51．0％，纯度99．3％；利用红外光谱、核磁共振、质谱、元素分析等手段对中间体与目标化合物的结构进行表征；探讨了氧化呋咱成环反应机理以及肟化、重氮化／脱氮及氧化呋咱成环的影响因素。氧化呋咱成环的最佳反应条件：Na2CO3摩尔量为理论值的1．10～1．25倍，反应温度2～10℃，反应时间4h，收率75．6％，纯度不小于99．0％（HPLC）。

3,4-Bis（pyrazine 2＇-yl）furoxan（DPF） was synthesized using 2 cyanopyrazine as raw material, via fourstep reactions of oxime, diazotization, denitrification and cyclization and the overall yield was 51. 0%. The structures of target compound and intermediates were characterized by IR, NMR, MS and elemental analysis. The mechanism of cyclization reaction was investigated. The affecting factors of reactions were optimized. The optimum reaction conditions of eyelization were： molar ratio nexp ： n theory ： 1. 10 -1. 25 for Na2CO3, reaction temperature 2 to 10℃ and reaction time 4h. The yield of DPF is about 75.6% and purity 99.0%.