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以对苯二甲酸和碘为原料,50%发烟硫酸为溶剂,制得2,3,5,6-四碘对苯二甲酸,再通过氯化亚砜进行酰氯化,最后与葡甲胺反应合成了标题化合物。其结构通过元素分析、红外光谱、核磁共振氢谱,质谱得到确证。运用正交实验优化了酰胺化反应条件:三乙胺为缚酸剂,四碘对苯二甲酰氯和葡甲胺为反应物,它们的物质的量比为2.1∶1∶2.4,反应温度为40℃时,产率高达71.5%。 相似文献
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以对苯二甲酸二酯与对苯二胺为原料,氢化钠为催化剂,合成了一种芳香性二酰胺二胺化合物.与其他对苯二甲酸二酯相比,对苯二甲酸二甲酯在40℃下有较高的活性,和对苯二胺反应生成N,N'-双(对氨基苯基)对苯二甲酰胺的产率在60%以上.反应产物的结构分别用元素分析,IR和1HNMR进行了表征. 相似文献
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以多聚磷酸与磷酸的混合酸为催化剂,由对苯二甲酸与邻苯二胺缩合,合成了1,4-双(2-苯并咪唑基)苯,收率为87.7%.通过各种试验,得到的优化反应条件为:催化剂中多聚磷酸与磷酸的体积比为1∶4,反应物料配比为n(对苯二甲酸):n (邻苯二胺)=1∶2.2,反应温度为200 ℃, 反应时间为6 h.产物经元素分析、IR谱、1HNMR谱表征,同时发现固体产物发射很强的紫色荧光,荧光寿命为0.52 ns.通过将稀土金属离子Er3+与1,4-双(2-苯并咪唑基)苯配位,大大改进其原有的荧光性质,Er(Ⅲ)配合物发射蓝色荧光,荧光强度增大到原化合物的3倍,荧光寿命也增加到0.99 ns. 相似文献
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为了制备高纯度与高收率的2,3,5,6-四氨基吡啶/2-羟基对苯二甲酸复合盐(TH盐),通过以2,6-二氨基-3,5二硝基吡啶(DADNP)为原料催化加氢还原制得2,3,5,6-四氨基吡啶盐酸盐(TAPH)。反应在55~60℃的氢气氛围下,以甲醇为溶剂,Pd/C为催化剂制得纯度99.4%的TAPH,收率82.1%。制成的盐酸盐再和2-羟基对苯二甲酸(HTA)钠盐在氮气氛围的保护下合成2,3,5,6-四氨基吡啶/2-羟基对苯二甲酸复合盐(TH盐)单体,结构经过13C-NMR、MS和FT-IR表征分析,结果表明是目的产物,纯度达98%以上。 相似文献
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以苯甲酰氯、四氯化碳、间甲基苯甲酰氰为原料,合成了标题化合物。重点考察了氰化过程中不同原料配比、反应温度、时间、溶剂和催化剂用量对收率的影响。实验结果表明,其最佳反应条件为:n(1,1,2-三氯-2-苯基乙烯)∶n(3-甲基苯甲酰氰)=1∶1.2,二氯甲烷为反应溶剂,3 mmol催化剂三乙胺,室温反应5 h,总收率达80.6%。 相似文献
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研究了2,2,3,3-四溴-1,4-丁二醇的合成方法,讨论了温度、溶剂、催化剂、反应时间、原料配比等因素对产品收率的影响,并提出了反应母液循环利用的有关问题。 相似文献
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以w(NaOH) =33%水溶液为催化剂、乙醇胺、丁酮和二氯乙酰氯为原料 ,一步法合成了3 二氯乙酰基 2 甲基 2 乙基 1,3 口恶唑烷。采用正交实验设计获得最佳反应条件 :三氯甲烷做溶剂 ,反应温度 - 4~ 4℃ ,反应搅拌时间 1h ,产物收率 78 6 %。产品经红外光谱、核磁共振和元素分析确证。 相似文献
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Silicon carbide ceramics (SiC) are used in different applications in the engineering area due to the excellent properties, mainly in high temperatures. They are usually obtained by liquid-phase sintering enabling to form volatile products and, consequently, defects. The present work aims at studying the obtention of SiC ceramics by spontaneous infiltration using a eutectic composition of the Al2O3/Y2O3, AlN/Y2O3, Al2O3/Sm2O3, AlN/Sm2O3, Al2O3/RE2O3 and AlN/RE2O3 systems. RE2O3 is the concentrate of the rare-earth oxide obtained from Xenotime ore. Infiltration tests were carried out in argon atmosphere, graphite crucibles, in several temperatures near the melting point of each system, varying from 2.5 to 60 min. It was observed that Al2O3/Y2O3, Al2O3/Sm2O3, AlN/Sm2O3 and Al2O3/RE2O3 systems do not infiltrate appropriately and the AlN/Y2O3 and AlN/RE2O3 systems infiltrated spontaneously more than 20 mm; however, the first one presented a higher degree of infiltration, approximately 97%. 相似文献
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以苯和戊二酸酐为原料,经取代反应、沃夫-黄鸣龙还原和环化脱水,制得2,3-苯并环庚酮,最优反应条件为:n(戊二酸酐)∶n(苯)∶n(三氯化铝)=1∶2∶2,室温反应3 h,溶剂为四氢呋喃;沃夫-黄鸣龙还原反应温度为160℃,反应时间为2 h;环化脱水反应温度为120℃,时间2 h,反应总收率60.3%,用IR、1HNMR、13CNMR及MS对中间体及目标产物结构进行了表征。 相似文献
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Active 4-dodecanoyl-2-nitrophenyl esters of β-alanine, β-alanyl-β-alanine, and β-alanyl-β-alanyl-β-alanine were prepared, and tried to polymerize in various solvents. Nonpolar solvents were found to be convenient for the polycondensation reaction. The yield of the polycondensation was high for the monopeptide ester, and less for the dipeptide and tripeptide esters. The effect of temperature on the polycondensation reaction was also studied. 相似文献
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Shunsuke Murakami Nihal Thafeem Ahmed Faheem Ahmed Dawei Wang Antonio Feteira Derek C. Sinclair Ian M. Reaney 《Journal of the European Ceramic Society》2018,38(12):4220-4231
A crystallochemical framework is proposed based on electronegativity difference (en) and tolerance factor (t) to optimise the BiMeO3 dopants and therefore the piezoelectric and high-field strain response in BaTiO3-BiFeO3 based ceramics. Compositions in the series 0.05Bi(Me)O3-0.25BaTiO3-0.7BiFeO3 (BMe-BT-BF, Me: Y, Sc1/2Y1/2, Mg2/3Nb1/3, Sc, Zn2/3Nb1/3, Zn1/2Ti1/2, Ga, and Al) were fabricated using solid state synthesis and furnace cooled. Scanning electron microscopy and X-ray diffraction revealed that only Bi(Mg2/3Nb1/3)O3 and BiScO3 dopants, which lie in a narrow range of en vs. t, form homogeneous ceramics, free from secondary phases reflected in their superior piezoelectric coefficients (d33 ~145 pC/N). All other BiMeO3 additions exhibited either secondary phases (Y) and/or promoted a two-phase perovskite matrix (Zn, Ga and Al). The promising initial properties of BiScO3 doped compositions prompted further studies on 0.05BiScO3-(0.95-x)BaTiO3-(x)BiFeO3 (BS-BT-BF, x?=?0.55, 0.60, 0.625, 0.65, and 0.70) ceramics. As x increased the structure changed from predominantly pseudocubic to rhombohedral, resulting in a transition from a relaxor-like to ferroelectric response. The largest d33* (465?pm/V) was achieved for x?=?0.625 under 5?kV/mm at the crossover from relaxor to ferroelectric behaviour. BS-BT-BF with x?=?0.625 showed >0.3% strain under 6?kV/mm up to 175?°C, demonstrating its potential for actuator applications. 相似文献