[1]王鹏程,刘想,陆明,等.2,3,5,6-四氨基吡啶盐酸盐的合成[J].南京理工大学学报(自然科学版),2012,36(05):898.
 WANG Peng-cheng,LIU Xiang,LU Ming,et al.Synthesis of 2,3,5,6-Tetraamineopyridine Hydrochloride[J].Journal of Nanjing University of Science and Technology,2012,36(05):898.
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2,3,5,6-四氨基吡啶盐酸盐的合成
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《南京理工大学学报》(自然科学版)[ISSN:1005-9830/CN:32-1397/N]

卷:
36卷
期数:
2012年05期
页码:
898
栏目:
出版日期:
2012-10-31

文章信息/Info

Title:
Synthesis of 2,3,5,6-Tetraamineopyridine Hydrochloride
作者:
王鹏程1刘想1陆明1熊贤锋2
1. 南京理工大学化工学院,江苏南京210094;2. 西安近代化学研究所,陕西西安710065
Author(s):
WANG Peng-cheng1LIU Xiang1LU Ming1XIONG Xian-feng2
1. School of Chemical Engineering,NUST,Nanjing 210094,China;2. Xi爷an Modern Chemistry Research Institute,Xi′an 710065,China
关键词:
硝基吡啶氨基吡啶硝化催化加氢
Keywords:
nitropyridinesaminopyridinesnitrificationcatalytic hydrogenation
分类号:
TJ55;O6
摘要:
为了研究2,3,5,6-四氨基吡啶的合成工艺,该文以2,6-二氨基吡啶为原料,通过硝化反应得到2,6-二氨基-3,5-二硝基吡啶,进一步加氢还原制得2,3,5,6-四氨基吡啶盐酸盐。研究发现:H2SO4-SO3 / HNO3 硝化体系反应温度30 益、反应时间3 h 时,2,6-二氨基-3,5-二硝基吡啶产率可达90%以上。实验比较了Fe、水合肼和催化加氢三种还原方法对2,6-二氨基-3,5-二硝基吡啶还原结果的影响。结果表明,催化加氢的效果最佳。在溶剂为乙醇、反应温度为50 益、反应压力为1. 0 ~1. 5 MPa、催化剂Raney Ni 质量为底物的10%条件下,2,3,5,6-四氨基吡啶酸盐酸的收率为89%,所用催化剂Raney Ni 经NaOH 溶液处理能循环使用4 次。
Abstract:
In order to study the synthetic technology of 2, 3, 5, 6-tetraaminopyridine, 2, 6-diaminopyridine is nitrated into 2,6-diamino-3,5-dinitropyridine which is reduced into 2,3,5,6-tet-raaminopyridine. The super-acid system is much better than the mixed acid. Under 30益temperatureand 3 h reaction time,the yield increases to 90%. The experiment results show that the Raney Nicatalytic hydrogenation is better reduction method than the hydrazine hydrate and Fe powder. Whenthe reaction solvent is ethanol,the reaction temperature is 50℃,the reaction pressure is 1. 0 ~1. 5MPa,and the amount of catalyst is 10%(mass percent in nitropyridine compounds),the yield of 2,3,5,6-tetraaminopyridine hydrochloric acid is 89%. The Raney Ni can be recycled for four timesafter treated with of sodium hydroxide solution.

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备注/Memo

备注/Memo:
收稿日期:2011-05-12修回日期:2011-12-04基金项目:国家自然科学基金委员会-中国工程物理研究院联合基金(11076017)作者简介:王鹏程(1985-),男,博士生,主要研究方向:含能材料制备与精细有机合成,E-mail:alexwpch@ 163.com;通讯作者:陆明(1963-),男,博士,教授,博士生导师,主要研究方向:含能材料制备与精细有机合成,E-mail: luming@ mail. njust. edu. cn。
更新日期/Last Update: 2012-11-26