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本研究测定了2-乙基己基膦酸单2-乙基己基酯与镧系元素镧、铈、镨、钕、钐、铕、钬、铒、镱、镥的^1H,^13C,^31P核磁共振谱,对HEH/EHP的碳骨架进行了详细归属,并根据^31P NMR谱峰的积分面积,推测了萃合物可能的配位络合比,对铕、镱、镥为6,对铒为5、对钬、钐为4。 相似文献
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ICP-AES法测定高纯氧化铕中稀土杂质元素 总被引:1,自引:0,他引:1
研究了锌粉还原 5709萃淋树脂分离富集 ICP AES法测定高纯氧化铕中14个稀土杂质元素的方法,用ICP AES法测定稀土元素工作曲线下限为(以氧化物计)镧为0.05mg·L-1,铈、镨、钇为0.25mg·L-1,钕、钐、铽、镝、钬为0.1mg·L-1,铒、铥、镱、镥、钇为0.05mg·L-1,回收率为90%~106%。方法简便、准确、快速,可用于99.99%氧化铕中14个稀土杂质元素的测定。 相似文献
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稀土氧化物上SO2和NO的催化还原 Ⅱ.用CO作还原剂的脱硫及反应机理 总被引:6,自引:2,他引:6
采用连续流动固定床石英反应器,在反应气体为1%SO2和2%CO,流量为180ml/min,以及催化剂用量为0.5g的条件下,考察了经活化处理的稀土系列氧化物对CO还原SO2的催化活性,探讨了空速、温度和水蒸气等因素对反应的影响,所研究的样品依据对SO2的转化能力可分为三组:高活性的镧、镨、钕、钐、铕和钆氧化物;低活性的铈、狄和铒氧化物;无活性的铽和氧化物,在活性最高的钕和钐氧化物样品上,450℃时SO2的转化率〉98%,反应过程中,活性相为稀土氧硫化物,反应遵从COS中间物机理。 相似文献
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稀土氧化物上SO2和NO的催化还原Ⅱ.用CO作还原剂的脱硫及反应机理 总被引:2,自引:0,他引:2
采用连续流动固定床石英反应器,在反应气体为1%SO2和2%CO, 流量为180 ml/min, 以及催化剂用量为0.5 g的条件下,考察了经活化处理的稀土系列氧化物对CO还原SO2的催化活性,探讨了空速、温度和水蒸气等因素对反应的影响.所研究的样品依据对SO2的转化能力可分为三组: 高活性的镧、镨、钕、钐、铕和钆氧化物; 低活性的铈、钬和铒氧化物; 无活性的铽和镝氧化物.在活性最高的钕和钐氧化物样品上, 450 ℃时SO2的转化率>98%.反应过程中,活性相为稀土氧硫化物,反应遵从COS中间物机理. 相似文献
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有机溶剂萃取钐、铕、铽与β-二酮、中性配体三元络合物荧光法测定钐、铕、铽已有报道;而在表面活性剂存在下,直接测定水相荧光的研究仍不多。为此,研究了乳 相似文献
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用溶胶-凝胶法以磷钼酸(MPA)的镍盐溶液水解钛酸四丁酯制备了NiPMo/TiO2催化剂.使用ICP、 XRD、 TG-DTA、 IR、 TPD-MS和微反应技术研究了催化剂的化学组成、热稳定性、化学吸附性质和催化反应性能.杂多钼酸盐与TiO2通过O2-在TiO2表面发生了键合.在623 K下,杂多阴离子仍保持原有的Keggin结构.CO2在Lewis酸位Ni(Ⅱ)和Lewis碱位Ni-O-Mo的桥氧协同作用下生成CO2卧式吸附态Ni(Ⅱ)←O-(CO)←(O--Ni).丙烯有多种吸附态在催化剂上吸附.在563 K、 1 MPa和空速1500 h-1的反应条件下,丙烯的摩尔转化率为3.2%,产物MAA选择性为95%. 相似文献
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Different approaches for the synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives from simple amino acids have been investigated. A library of 33 precursors for the preparation of N-hydroxy pyrazinones was obtained in moderate to good yields. 相似文献
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Toward new camptothecins. Part 6: Synthesis of crucial ketones and their use in Friedländer reaction
Laurent Gavara Thomas Boisse Jean-Pierre Hénichart Adam Daïch Philippe Gautret 《Tetrahedron》2010,66(38):7544-5571
In the context of the preparation of camptothecin and luotonin A analogs, the synthesis of some key keto-precursors and their use in Friedländer condensation are described. This paper also focuses on the stability of these keto intermediates and emphasizes the major differences between indolizinones and pyrroloquinazolinones series. Noteworthy is also the report of some original structures isolated as by-products of some experiments. 相似文献
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The Langevin paramagnetic theory can’t describe the relation between magnetization of ferrofluids and applied magnetic field. The structuralization of ferrofluids, which is considered the main influence factor of the magnetization, is regarded. The part of magnetization works is deposited when the structure is forming. This action influences the magnetization of ferrofluids directly or indirectly. On the base of the “compressing” model, the Langevin function that usually describes the magnetization of ferrofluid is modified, and a well-fitted curve is obtained. An equation of the relation between the equivalent volume fraction after being “compressed” and the intensity of magnetic field is discovered, which approximately describes the process of magnetization. The relation between the approximate initial susceptibility and the volume fraction can be obtained from modified formula. 相似文献
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Rebecca J. Burton Mandy L. CrowtherNeal J. Fazakerley Shaun M. FilleryBarry M. Hayter Jason G. KettleCaroline A. McMillan Paula PerkinsPeter Robins Peter M. SmithEmma J. Williams Gail L. Wrigley 《Tetrahedron letters》2013
The highly regioselective Buchwald–Hartwig amination at C-2 of the cheap and readily accessible reagent, 2,4-dichloropyridine with a range of anilines and heterocyclic amines is described. This new methodology is robust and provides a facile access to 4-chloro-N-phenylpyridin-2-amines on 0.25 mol scale. These intermediates undergo a further Buchwald–Hartwig amination at higher temperature to enable rapid exploration of the chemical space at C-4 and to provide a library of 2,4-bisaminopyridines. 相似文献
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KMnO4-mediated oxidative CN bond cleavage of tertiary amines producing secondary amine was introduced, which was trapped by electrophiles (acyl chloride and sulfonyl chloride) to form amides and sulfonamides. The reaction could take place at mild condition, tolerating a wide range of function groups and affording products in moderate to excellent yields. 相似文献
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N. A. Nedolya 《Chemistry of Heterocyclic Compounds》2008,44(10):1165-1219
The review contains a concise historical account and information on the most significant researches undertaken by the staff
at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences on the Chemistry
of Heterocyclic Compounds.
Dedicated to Academician of the Russian Academy of Sciences B. A. Trofimov on his 70th jubilee.
Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 10, pp. 1443–1502, October, 2008. 相似文献
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A general synthesis of previously unknown semicarbazone-based α-amidoalkylating reagents, 4-(tosylmethyl)semicarbazones, has been developed. The synthesis involved three-component condensation of semicarbazones of aliphatic or aromatic aldehydes with the same or other aldehydes and p-toluenesulfinic acid. The scope and limitations of this reaction were investigated. The compounds obtained were demonstrated to be an efficient α-(4-semicarbazono)alkylating agents. They were reacted with H- (sodium borohydride), O- (sodium methylate), S- (sodium phenylthiolate), N- (pyrrolidine, sodium succinimide), P- (trialkyl phosphites), and C-nucleophiles (sodium diethyl malonate) to give the corresponding products of the tosyl group substitution, 4-substituted semicarbazones, including analogues of nitrofurazone. Among the prepared compounds tested in vitro for antibacterial and antifungal activity, three nitrofuryl-containing semicarbazones exhibited high biological activities with minimum inhibitory concentration (MIC) values of 8–32 μg/mL. 相似文献
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Regiospecific and direct imidation of the methyl C(sp3)–H bond of thioanisoles is realized under mild and metal-free conditions with N-fluorobis(benzenesulfonyl)imide as an oxidant and nitrogen source. Proposed mechanism suggests that thionium ion intermediates and a Pummerer-type reaction are involved. The imidation has advantages such as high step-economy, excellent functionality tolerance, and regiospecificity, giving structurally diverse imidation products. 相似文献
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A small library of new chiral bidentate hydroxyalkyl-imidazolium salts 1 is conveniently synthesized on multi-gram scale from inexpensive and commercially available chiral pool amino acids. The corresponding carbenes, generated by deprotonation of imidazolium salts 1, in combination with palladium(II) chloride were tested in the Mizoroki–Heck coupling reaction. The most significant results in terms of yields and reactivities were achieved with low catalyst loading. The catalytic activities of these imidazolium salts were also investigated in the asymmetric addition of diethylzinc to benzaldehyde. The use of MgO nanoparticles as an additive in conjunction with these ligands played a crucial role in increasing the efficiency of these reactions. 相似文献