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1.
四烃基二锡氧烷在酯化反应中的催化作用 总被引:4,自引:0,他引:4
1,1,3,3-四烃基二锡氧烷Ⅰ是一类有机锡氧簇合物,它在固相和液相中[1,2]均为二聚梯形层状结构,在有机合成中表现出特殊的催化活性,与其它含Sn—O键非簇类化合物相比,催化活性和选择性均有大幅度提高.该类化合物是酯交换、酯化、官能团保护和脱保护等反应的优良催化剂[3].本文合成了一系列四烃基二锡氧烷,并以乙酸与丁醇的酯化反应为例,研究其对该反应的催化作用. 相似文献
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三苄基锡羧酸酯的合成 总被引:3,自引:0,他引:3
合成了三苄基锡苯甲酸酯,三苄基锡水扬酸酯,三苄基锡3-羟基-4-羧基苯磺酸酯和三苄基锡对氯苯氧乙酸酯4种化化合物,对其进行了IR,1H NMR表征,发现苯甲酸,水扬酸和对氯苯氧乙酸与三苄基锡氧化物反应生成三苄基锡羧酸酯,而对磺基水杨酸与三苄基锡氧化物反应生成三苄基锡3-羟基-4-羧基苯磺酸酯,4种化合物对苯甲醛,庚醛和乙二醇缩合反应的催化活性测试表明,其活性次序为:三苄基锡3-羟基-4-羧基苯磺酸酯>三苄基锡水杨酸酯>三苄基锡苯甲酸酯>三苄基锡对氯苯氧乙酸酯。 相似文献
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有机锡氧簇合物在有机合成中的催化作用 总被引:10,自引:0,他引:10
综述了以四烃基二锡氧烷Ⅰ为代表的有机锡氧簇合物作为催化剂在酯交换、酯化、羰基缩醛保护和脱保护以及开环聚合等有机反应中的催化作用。化合物Ⅰ的Sn-O环具有独特的二聚层状结构,使其在有机合成中体现出特殊的催化活性。本文就相关反应和反应机理进行了综述。 相似文献
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Ni/Al2O3催化剂上CH4部分氧化制合成气反应积碳的原因 总被引:7,自引:0,他引:7
采用程序升温在线质谱分析方法,研究了常压条件下CH4在Ni/Al2O3催化剂上分解所形成的碳物种,发现CH4分解形成的NixC会首先转化成不与CO2反应,但在700℃左右可与O2反应的碳;这种碳再向需在800℃才能与O2反应的石墨碳转化.在较低的温度下,NixC向石墨碳转化的速度较慢,而在高温条件下转化速度大大加快.在700℃下,Ni/Al2O3催化剂上的CH4部分氧化制合成气反应生成的积碳主要为石墨碳,是由CH4分解形成的NixC转化而成的.在催化剂中添加适当的助剂,可提高NixC与氧的反应活性,抑制其向石墨碳转化,是改善催化剂抗积碳性能的有效途径. 相似文献
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通过氧化二烃基锡与二氯二烃基锡的反应,合成了不对称四烃基二锡氧烷[ClR2SnOSnR'2Cl]2 (R=Bu,Pr; R'=Me,Ph,Cy,Oct).通过对化合物1和5的X-衍射晶体结构分折,表明该类化合物在晶体状态 时是含有中心对称Sn2O2四元环的梯状二聚体,内环锡与外环锡均为五配位的畸变三角双锥构型. 相似文献
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四丁基二锡氧烷催化合成碳酸二酯类化合物的新方法 总被引:12,自引:0,他引:12
以四丁基二锡氧烷为催化剂,通过尿素的醇解反应,合成了四种\r\n高沸点碳酸二酯化合物.研究结果表明,尿素的第一步醇解反应较易进\r\n行,产物收率大于60%;第二步从氨基甲酸酯醇解变为碳酸二酯的反应\r\n较难进行.尿素醇解反应与所用的醇有密切的关系,其中尿素与苯甲醇\r\n醇解为碳酸二酯的反应最易进行,正己醇次之,而正辛醇反应最难进行\r\n.提高反应温度到195℃,以官能团为NCS的四丁基二锡氧烷代替官能团\r\n为Cl的四丁基二锡氧烷为催化剂时,适当提高醇的配比,尿素与正辛醇\r\n醇解为碳酸二酯的产物收率有较大的提高.提出了尿素醇解反应的可能\r\n机理. 相似文献
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Ni/Al2O3催化剂上CH4发氧化制合成气反应积炭的原因 总被引:1,自引:0,他引:1
采用程序升温在线质谱分析方法,研究了常太条件下CH4在Ni/Al2O3催化剂上分解所形成的碳物种,发现CH4分解形成的NixC会首先转化成不与CO2反应,但在700℃左右可与O2反应的碳;这种碳再向需在800℃才能与O2反应的石墨碳转化,在较低的温度下,NixC向石墨碳转化的速度较慢,而在高温条件下转化速度大大加快,在700℃下,Ni/Al2O3催化剂上的CH4部分氧化制合成气反应生成的积炭主要为石墨碳,是由CH4分解形成的NixC转化而成的,在催化剂中添加适当的助剂,可提高NixC与氧的反应活性,抑制其向石墨碳转化,是改善催化剂抗积碳性能的有效途径。 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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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 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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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