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为降低HNIW的合成成本,节省钯催化剂用量,以六苄基六氮杂异伍兹烷(HBIW)的一次氢解产物四乙酰基二苄基六氮杂异伍兹烷(TADBIW)作为反应基质,采用市售无机试剂使TADBIW分子上的两个苄基脱掉,实现了无钯脱苄的目的,分别合成出了四乙酰基二亚硝基六氮杂异伍兹烷(TADNSIW)和四乙酰基二硝基六氮杂异伍兹烷(TADNIW),得率分别为80.0%和70.6%;由TADNSIW经氧化、硝化合成了六硝基六氮杂异伍兹烷(HNIW),得率为96.2%,HNIW的纯度达到98.0%以上;由TADNIW和100%硝酸反应合成HNIW,得率为96.0%,纯度高于98.0%;由TADBIW采用一锅煮合成了HNIW,得率为82.2%,纯度在98.0%以上。
Abstract:To reduce the cost for producing hexanitrohexaazaisowurtzitane ( HNIW), inorganic materials available from market readopted to remove two benzyls to prepare tetraacetyldinitrosohexaazaisowurtzitane (TADNSIW)and tetraacetyldinitrohexaazaisowurtzitane(TADNIW)as the precursors for synthesizing HNIW from tetraacetyldibenzylhexaazaisowurtzitane(TADBIW), with the yield of 80.0% and 70.6% respectively. HNIW is synthesized from TADNSIW with the yield of 96.2% and 96.0% respectively,and with the purity of higher than 98.0% .Preparation of HNIW from TADBIW can be also performed by one- pot method in larger scale,with the yield of 82.2% and purity higher than 98.0% .
[1] Olah A G,Square D R.Chemistry of Energetic Materials[M].San Diego:Academic Press Inc,1991. 95.
[2] 徐更光.汪旭光,于永忠.中国高能量密度材料的研究与应用[M].上海:上海教育出版社,1997. 288.
[3] 欧育湘,徐永江,陈江涛等.高张力笼形氮杂环化合物的合成[J].高等学校化学学报,1999,20(4) :561~564.
[4] Tamotsu Kodama,Haruyuki Minoura,Nobuhisa,et al. Process for the Preparation of Acylated Hexaazaisowutzitane Derivatives[P]. US:6153749,2000-11-28.
[5] Anthony J.Bellamy. Reductive Debenzylation of Hexabenzylhexaazaisowurtzitane. Tetrahedron, 1995,51(6) :4711-4722.
[6] Arnold T.Nielsen,Andrew P. Chafin,Stephen L. Christian,et al. Synthesis of Polyazapolycyclic Caged Polynitramines[J]. Tetrahedron, 1998,54(16) :11793-11812.
[7] 于永忠,管晓培.六硝基六氮杂异伍兹烷的合成研究[J].含能材料,1999,7(1) :1~4
[8] Nikolaj V.Latypov.Ulf Wellmar,Patrick Goede,et al. Synthesis and Scale-up of 2,4,6,8,10,12-hxanitro-2,4,6,8,10,12-hexaazaisowurtz-itane from 2,6,8, 12-Tetraacetyl-4, 10-dibenzyl-2,4,6,8, 10, 12-hexaazaisowurtzitane ( HNIW, CL-20) [J]. Organic Process Research&Development,2000,4(3) : 156-158.
[9] 孙荣康,任特生,高怀林.猛炸药的化学与工艺学[M].北京:国防工业出版社,1981. 11.
[10] 邢其毅,徐瑞秋,周政等.基础有机化学[M].北京:高等教育出版社,1993. 595.
基本信息:
中图分类号:TQ560
引用信息:
[1]吕连营,欧育湘,次立杰,王建龙.由TADBIW合成HNIW[J].石家庄师范专科学校学报,2003(06):4-8.
基金信息:
国防科工委预研基金资助项目(12060451867)
2003-11-20
2003-11-20