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不同载体钯催化剂的结构表征及其在笼形叔胺脱N-苄基上的应用 总被引:1,自引:1,他引:0
以γ Al2O3、木质活性炭、煤质活性炭为载体,以氯化钯为前体制备了Pd(OH)2/Al2O3、Pd(OH)2/C催化剂,并用X射线衍射、透射电镜和X射线光电子能谱等技术对这些催化剂进行了结构表征。以六苄基六氮杂异伍兹烷(HBIW)的脱苄反应为例,研究了不同载体Pd(OH)2催化剂对笼形叔胺N 苄基脱苄反应的活性,分析了影响催化剂活性的各种因素。实验结果表明,当催化剂用量为HBIW质量的0 2%(以Pd计)时,氢解产品四乙酰基二苄基六氮杂异伍兹烷(TADBIW)的收率可达88%,其中以煤质活性炭为载体的催化剂已用于HBIW氢解脱苄的20kg级放大实验,TADBIW产品收率为82%。 相似文献
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Tetraacetyldibenzylhitane (TADBIW) was subjected to debenzylation by nitrosating with inorganic materials available commercially to synthesize tetraacetyldinitrosohexaazaisowurtzitane (TADNSIW). TADNSIW was purified, and its structure was determined by FTIR, 1H NMR, MS and element analysis. The debenzylation reaction of TADBIW gave quantitative benzaldehyde as a by-product. This indicates that the reaction produces an imine cation as an intermediate. Hexanitrohexaazaisowurtzitane (HNIW) was prepared from unpurified TADNSIW with the yield over 96.0 % and the purity more than 98.0 %. And the mechanism of the reaction from TADNSIW to HNIW is proposed to be oxidation of nitroso and nitration of acetyl on the molecule of TADNSIW, This reaction system involved is simple, and the reaction can complete within a short time and under mild conditions. The product can be easily to separate and the waste disposed readily. 相似文献
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本文叙述了三个化合物5-甲胺基-2,4-二硝基叠氮苯(Ⅰ)、5-甲硝胺基-2,4,6-三硝基叠氮苯(Ⅱ)及5-甲胺基-4,6-二硝基苯并氧化呋咱(Ⅲ)的合成。通过对核磁共振氢谱的分析,确定了化合物(Ⅰ)与(Ⅲ)分别以一对几何异构体存在。本文中还对化合物(Ⅲ)的某些性质作了报告。 相似文献
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Hexabenzylhexaazaisowurtzitane (HBI W) is thefirst precursor of synthesizingthe high energy densitycaged nitramine 2 ,4 ,6 ,8 ,10 ,12-hexanitro-2 ,4 ,6 , 8 , 10 , 12-hexaazatetracyclo-[5 .5 .0 .05 ,9.03 ,11]-dodecane (HNI W)[1 -3]. HBI Witself is likely to beunstable in most solvents and easily to be decomposedeventhoughin weaker acid medium.Direct nitration-debenzylation of HBI Wis unlikely to be successfuldue to both competing nitration of phenyl rings andinstability of the ring system… 相似文献
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