3,3'-二氨基-4,4'-氧化偶氮呋咱的合成  

Synthesis of 3,3'-Diamino-4,4'-axoxyfuranzan

作　　者：刘燕[1] 安崇伟[1] 王晶禹[1] LIU Yan AN Chong-wei WANG Jing-yu(School of Chemical Engineering and Environment, North University of China, Taiyuan 030051, China)

机构地区：[1]中北大学化工与环境学院,山西太原030051

出　　处：《合成化学》2016年第10期899-902,共4页Chinese Journal of Synthetic Chemistry

摘　　要：以3,4-二氨基呋咱(DAF)为初始原料,用硝硫混酸-双氧水催化氧化体系代替了原来的浓硫酸-双氧水氧化体系,经一步法高效氧化合成了3,3'-二氨基-4,4'-氧化偶氮呋咱(DAOAF),其结构经1H NMR,FT-IR和元素分析确证。在最佳反应条件[DAF 0.01 mo L,硝硫混酸10 m L(30 min内滴毕),H2O212 m L,于20℃反应20 h]下,DAOAF收率和纯度分别为96.8%和99.2%。采用差示扫描量热法(DSC法)对其热稳定性进行了分析。结果表明:DAOAF的初始分解温度为250℃。3,3＇-Diamino4, 4＇-axoxyfuranzan （ DAOAF ） was synthesized from 3,4-diaminofurazan （ DAF）, using a new catalytic oxidation system of mixed acid-hydrogen peroxide replacing the original catalytic oxidation system of sulfuric acid-hydrogen peroxide. The structure was confirmed by I H NMR, FT-IR and elemental analysis. The results showed that the yield and purity reached to 96.8% and 99.2% under the optimum reaction conditions[ DAF 0.01 mol, the mixed acid 10 mL （dripped off in 0.5 h） and H2 02 12 mL, reaction at 20℃ for 20 h ]. The thermal stability of DAOAF was ana- lyzed by DSC. The results showed that the initial decomposition temperature was 250℃.

关 键 词：3 4-二氨基呋咱 3 3'-二氨基-4 4'-偶氮氧化呋咱 氧化 一步法 合成 

分 类 号：O626[理学—有机化学]