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[1]罗军,李娅琼.用改进的Sollott法合成1,3,5,7-四硝基金刚烷[J].火炸药学报,2011,34(5):13-15.
 LUO Jun,LI Ya-qiong.Synthesis of 1,3,5,7-Tetranitroadamantane via Modified Sollott′s Route[J].,2011,34(5):13-15.
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用改进的Sollott法合成1,3,5,7-四硝基金刚烷()
     
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《火炸药学报》[ISSN:1007-7812/CN:61-1310/TJ]

卷:
34
期数:
2011年第5期
页码:
13-15
栏目:
出版日期:
2011-10-31

文章信息/Info

Title:
Synthesis of 1,3,5,7-Tetranitroadamantane via Modified Sollott′s Route
作者:
罗军李娅琼
南京理工大学化工学院
Author(s):

LUO Jun LI Ya-qiong

School of Chemical Engineering, Nanjing University ofScience and Technology, Nanjing 210094, China
关键词:
有机化学1357-四硝基金刚烷溴化碘化酰胺化氧化
Keywords:

organic chemistry 1357-tetranitroadamantane brominationiodation amidation oxidation

分类号:
-
DOI:
-
文献标志码:
A
摘要:
以金刚烷为原料经过溴化、卤素交换碘化、酰胺化、水解和氧化5步反应合成1,3,5,7-四硝基金刚烷(TNA)。其中,第三步自由基酰胺化反应用偶氮二异丁腈(AIBN)在常规玻璃仪器中进行化学引发,代替了Sollott法中用石英反应瓶和特殊的Ryaonet光化学反应器的光照引发。结果表明,该方法的反应时间从64h缩短到30min,1,3,5,7-四乙酰氨基金刚烷的产率从51%提高到95%;TNA的总产率从文献报道的8%提高到18%。
Abstract:

1,3,5,7 -Tetranitroadamantane (TNA) was prepared fromadamantane via a five-step route: bromination, halogen-exchange iodation,amidation, hydrolysis and oxidation. The third step, free radical amidation,was catalyzed by AIBN in common glassware instead of photolyzed by ultravioletin quartz reaction flask and Rayonet photochemical reactor in sollotts method. Theresults show that the reaction time could be dramatically shortened from 64h to30min, and the yield of 1,3,5,7 tetraacetamidoadamantane could bepromoted from 51% to 95%.The total yield of TNA from adamantane was promoted to18% against 8% reported in reference.

参考文献/References:

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