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微波辐射条件下,以氨基均三唑硫醇与查尔酮为原料,通过亲核取代反应,制备了3-(4-氨基-5-巯基-3-对甲苯基均三唑-1-氮代)-1,3-二苯-1-丙酮(3),(3)与系列芳香醛经缩合反应,合成了4种三唑硫酮席夫碱(4a-4d).探讨了各实验因素对收率的影响,得到了优化的工艺条件:n(芳香醛)∶n(氨基三唑硫酮)=1∶1.1微波功率500W,催化剂冰醋酸2mL,反应时间4-7min,溶剂DMF,收率为65%-77%.利用IR、MS、1H NMR对目标产物进行了结构表征. 相似文献
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磺化甲苯膦酸锆的制备及催化反应研究 总被引:4,自引:0,他引:4
首次制得磺化甲苯膦酸锆(ZSTP),用X-衍射、热重量分析、红外光谱、元素分析等进行了表征。并以磺化甲苯膦酸锆为固体酸催化剂对酯化、缩醛、缩酮、醇脱水成醚、成烯等有机反应进行了研究。ZSTP催化的反应收率高,操作简便,后处理容易,催化剂可以重复使用和再生。 相似文献
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Copolymer of styrene with 4-oxe-4(P-hydroxyl phenylamino) but-2-enoic acid (PSHPEA) and its luminescent lanthanide complexes Ln-PSHPEA (Ln = La, Eu, Tb and Y) were synthesized and characterized by means of elemental analysis, FT-IR, thermogravimetric analysis and fluorescence determination. The results showed that the carboxylic groups on the chain of the copolymer acted as bidentate ligands coordinated to lanthanide ions, but the amido carbonyl groups, amino N and hydroxy groups had not taken part in coordination; the coordination degree of -COO−/Ln3+ which determined the content of metal ions in the macromolecular complexes, was closely dependent on both the pH value of the solution and the molar ratio of St to 4-oxe-4(P-hydroxyl phenylamino) but-2-enoic acid in the polymer ligand. The fluorescence determination showed that the complexes exhibited characteristic fluorescence with comparatively high brightness and good mono-chromaticity. Typical relationship between emission intensity and Ln3+ ions content in macromolecular complexes exhibited some extent of fluorescence concentration quenching in our studies. The emission intensity of Tb-PSHPEA complexes was much stronger than that of Eu-PSHPEA complexes, which was attributed to especial effectivity in transferring energy from the lowest triplet energy level of the ligand onto the excited state (5D0) of Tb3+ ion than that (5D4) of Eu3+ ion. 相似文献
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研究了氢氧化钠介质皂化条件下,用草酸溶液从负载铈的P507有机相中直接反萃取沉淀铈的试验结果。利用红外光谱(IR)、X射线衍射(XRD)、扫描电子显微镜(SEM)及热重-差热分析仪(TG-DSC)等手段,对反萃所得铈沉淀物及最终焙烧产物的物相、形貌和热失重等进行了分析、测试与表征。实验结果表明:沉淀有机相为球形有机铈的配合物,焙烧产物为球形的立方晶系的CeO2晶体,说明前驱物与产物形貌有遗传继承性。IR证实了萃合物的结构与最终CeO2晶体结构完全不同,热重表明吸附水失重为3.5%,所得最终产物的化学组成为CeO2.1/3H2O。 相似文献
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