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101.
102.
5-硝基-6-羟基-2-(对甲氧羰基苯基)苯并噁唑的合成 总被引:1,自引:0,他引:1
研究了以关键中间体4-氨基-6-硝基间苯二酚盐酸盐(ANR·HCl)和对苯二甲酸单甲酯(MTA)为原料,分别经酰氯化、缩合、环合分步或原位合成AB型新单体前体--4-(5-硝基-6-羟基-2-苯并噁唑基)苯甲酸甲酯(MNB)的技术。 反应优化条件:在甲基异丁基酮溶剂中,n(ANR·HCl)∶n(MTA)=1.00∶1.03,115 ℃缩合反应2.5 h;m(ANR·HCl)∶m(PPA)=1.00∶3.25的多聚磷酸(PPA),120 ℃环合8.5 h;MNB收率75.68%(以ANR·HCl计),HPLC测定ω(MNB)=96.32%。 产物结构经1H NMR和IR确证。 相似文献
103.
Giuseppe Romanazzi Valentina Petrelli Ambra Maria Fiore Piero Mastrorilli Maria Michela DellAnna 《Molecules (Basel, Switzerland)》2021,26(4)
Recently, N-substituted anilines have been the object of increasing research interest in the field of organic chemistry due to their role as key intermediates for the synthesis of important compounds such as polymers, dyes, drugs, agrochemicals and pharmaceutical products. Among the various methods reported in literature for the formation of C–N bonds to access secondary anilines, the one-pot reductive amination of aldehydes with nitroarenes is the most interesting procedure, because it allows to obtain diverse N-substituted aryl amines by simple reduction of nitro compounds followed by condensation with aldehydes and subsequent reduction of the imine intermediates. These kinds of tandem reactions are generally catalyzed by transition metal-based catalysts, mainly potentially reusable metal nanoparticles. The rapid growth in the last years in the field of metal-based heterogeneous catalysts for the one-pot reductive amination of aldehydes with nitroarenes demands for a review on the state of the art with a special emphasis on the different kinds of metals used as catalysts and their recyclability features. 相似文献
104.
A magnetically heterogeneous CoFe2O4@SiO2-NH2-CoII nanoparticle was synthesized by the immobilization of Co (II) complex onto CoFe2O4@SiO2 nanoparticles, and the heterogeneous magnetic nanocatalyst was characterized by XRD, TEM, TGA, EDX, and FT-IR techniques. Then, the green and reusable method was introduced for a multicomponent synthesis of 1,4-dihydropyridine derivatives via Hantszch reaction. The synthesis of 1,4-dihydropyridine derivatives was proceeded by the reaction of aldehyde, ethyl acetoacetate, and ammonium acetate in the presence of this magnetic nanocatalyst in EtOH/Water (1:1). Simple work-up, short reaction times, excellent yields (60–96%) as well as green solvent are some advantages of this novel approach, and the corresponding products were purified with no need for chromatographic separation. 相似文献
105.
Kei Usui Prof. Dr. Yuichi Manaka Prof. Dr. Wang-Jae Chun Prof. Dr. Ken Motokura 《Chemistry (Weinheim an der Bergstrasse, Germany)》2022,28(5):e202104001
In this study, a novel Rh–iodide complex was synthesized through a surface reaction between an immobilized Rh cyclooctadiene complex and alkylammonium iodide (N+I−) on SiO2. In the presence of ammonium cations, the SiO2-supported Rh–iodide complex could be effectively used for the one-pot synthesis of various silylcarbonate derivatives starting from epoxy olefins, hydrosilanes, and CO2. The maximum turnover numbers (TONs) for the hydrosilylation reaction and the CO2 cycloaddition were 7600 (Rh) and 130 (N+I−), respectively. The catalyst exhibited much higher performance for hydrosilylation than solely the Rh complex on SiO2. The mechanism of the Rh-catalyzed hydrosilylation reaction and the local structure of Rh, which is affected by the co-immobilized N+I−, were investigated by using Rh and I K-edge XAFS and XPS. Analysis of the XAFS profiles indicated the presence of a Rh−I bond. The Rh unit was in its electron-rich state. Curve-fitting analysis of the Rh K-edge EXAFS profiles suggests dissociation of the cycloocta-1,5-diene (COD) ligand from the Rh center. Results from spectroscopic and kinetic analyses revealed that the high activity of the catalyst (during hydrosilylation) could be attributed to a decrease in steric hindrance and the electron-rich state of the Rh. The decrease in the steric hindrance could be attributed to the absence of COD, and the electron-rich state promoted the oxidative addition of Si−H. To the best of our knowledge, this is the first example of a one-pot silylcarbonate synthesis as well as a determination of a novel surface Rh–iodide complex and its catalysis. 相似文献
106.
Huy Tran Guillaume Revol Alyson Poyser Louis Barriault 《Angewandte Chemie (Weinheim an der Bergstrasse, Germany)》2022,134(1):e202110575
A one-pot cascade sequence to generate synthetically challenging polycyclic scaffolds is reported utilizing a novel Lewis acid gold catalyst for the key cyclization step, enabling the divergent synthesis of both 6,6,5-tricyclic and 6,6,6,5-tetracyclic cores through both ligand and reaction condition control. We have combined the intrinsic complexity and stereoselectivity of cycloadditions with the electronic and steric properties of gold complexes to selectively generate complex polycyclic scaffolds in a single operation. 相似文献
107.
Copper is found to be an effective catalyst for the preparation of alkynylphophonates. A novel copper-catalyzed one-pot synthesis of alkynylphophonates from terminal alkynes and dialkyl phosphites is developed which involves the haloalkynes intermediates. This method provides a unique and alternative approach to the well-documented oxidative coupling or arylpropiolic acid strategies. 相似文献
108.
AbstractMagnetic nanoparticles containing mesoporous carbon materials have been synthesized via an one-pot strategy associated with a direct carbonization process from resol, metal ion sources (Co(NO3)2·6H2O, Ni(NO3)2·6H2O) and triblock copolymer F127. The samples exhibited well-ordered 2-dimensional (2-D) hexagonal mesostructures with p6mm symmetry. The Brunauer-Emmet-Teller (BET) surface area and pore size 1.0wt%Co- and 1.0wt%Ni-FDU-15(700) with 1.0?wt% Co and 1.0?wt% Ni content were 700, 528 m2/g and 17.2, 36.4 Å, respectively, after carbonization at 700?°C. The saturation magnetization values of 1.0wt%Co- and 1.0wt%Ni-FDU-15(700) after carbonization at 700?°C were 1.3 and 1.0?emu/g, respectively. 相似文献
109.
Chi-Ta Lee Dr. Helan Wang Ming Zhao Dr. Tung-Han Yang Dr. Madeline Vara Prof. Dr. Younan Xia 《Chemistry (Weinheim an der Bergstrasse, Germany)》2019,25(20):5322-5329
The rational design and implementation of a one-pot method is reported for the facile synthesis of Pd@PtnL (nL denotes the number of Pt atomic layers) core-shell icosahedral nanocrystals in a single step. The success of this method relies on the use of Na2PdCl4 and Pt(acac)2 as the precursors to Pd and Pt atoms, respectively. Our quantitative analysis of the reduction kinetics indicates that the PdII and PtII precursors are sequentially reduced with a major gap between the two events. Specifically, the PdII precursor is reduced first, leading to the formation of Pd-based icosahedral seeds with a multiply-twinned structure. In contrast, the PtII precursor prefers to take a surface reduction pathway on the just-formed icosahedral seeds. As such, the otherwise extremely slow reduction of the PtII precursor can be dramatically accelerated through an autocatalytic process for the deposition of Pt atoms as a conformal shell on each Pd icosahedral core. Compared to the conventional approach of seed-mediated growth, the throughput for the one-pot synthesis of Pd@PtnL core-shell nanocrystals can be increased by more than 30-fold. When used as catalysts, the Pd@Pt4.5L core-shell icosahedral nanocrystals show specific and mass activities of 0.83 mA cm−2 and 0.39 A mgPt−1, respectively, at 0.9 V toward oxygen reduction. The Pt-based nanocages derived from the core-shell nanocrystals also show enhanced specific (1.45 mA cm−2) and mass activities (0.75 A mgPt−1) at 0.9 V, which are 3.8 and 3.3 times greater than those of the commercial Pt/C, respectively. 相似文献
110.
A simple and powerful one-pot reaction method was developed for the synthesis of heteracalixaromatics. In the presence of a base, one-pot macrocyclic condensation reaction between cyanuric chloride and 1,3-phenylene diols and diamines proceeded effectively under very mild conditions to afford a number of functionalised oxygen and nitrogen-bridged calix[2]arene[2]triazines in 33–54% yields. The method was applied in a multigram-scale (14.4 g) preparation of tetraoxacalix[2]arene[2]triazine. 相似文献