Three new mononuclear group 12 complexes with benzimidazole

Three iso-structural Zn(II), Cd(II), and Hg(II) complexes with 1-benzyl-2-phenyl-1H-benzimidazole (BPB), ZnBPB, CdBPB, and HgBPB, respectively, were synthesized by reaction of the ligand with the corresponding metal chlorides in methanolic solutions. The complexes [MCl2(BPB) 2], where M = Zn(II), Cd(II), or Hg(II), were characterized by elemental analysis, 13C, 1H, and [1H- 15N] heteronuclear multiple bond coherence NMR measurements, and Raman spectroscopy. The structures of the cadmium and mercury complexes were solved by single-crystal X-ray diffraction, while the structure of the zinc complex was determined by X-ray powder diffraction. The three compounds crystallize in the triclinic system in P-1 space group with the metal ions lying in a distorted tetrahedral environment. The zinc complex shows high luminescence in the solid state at room temperature. © 2014 Taylor and Francis.67813801391Sondhi, S.M., Rani, R., Singh, J., Roy, P., Agarwal, S.K., Saxena, A.K., (2010) Bioorg. Med. Chem. Lett., 20, p. 2306Andrzejewska, M., Yepez-Mulia, L., Cedillo-Rivera, R., Tapia, A., Vilpo, L., Vilpo, J., Kazimierczuk, Z., (2002) Eur. J.Med. Chem., 37, p. 973Ünal, A., Eren, B., (2013) Spectrochim. Acta A-M, 114, p. 129Ansari, K.F., Lal, C., (2009) Eur. J. Med. Chem., 44, p. 4028Labarbera, D.V., Skibo, E.B., (2005) Bioorg. Med. Chem., 13, p. 387Küçükbay, H., Durmaz, R., Orhan, E., Günal, S., (2003) Farmaco, 58, p. 431Navarrete-Vázquez, G., (2001) Bioorg. Med. Chem. Lett., 11, p. 187Mota, V.Z., Carvalho, G.S.G., Silva, A.D., Sodre-Costa, L.A., MacHado, P.A., Coimbra, E.S., Ferreira, C.V., Cuin, A., (2014) BioMetals, 27, p. 183Cheng, J., Xie, J., Luo, X., (2005) Bioorg. Med. Chem. Lett., 15, p. 267Nozary, H., Piguet, C., Tissot, P., Bernardinelli, G., Bünzli, J.C.G., Deschenaux, R., Guillon, D., (1998) J. Am. Chem.Soc., 120, p. 12274Elhabiri, M., Scopelliti, R., Bünzli, J.C.G., Piguet, C., (1999) J. Am. Chem. Soc., 121, p. 10747Muller, G., Bünzli, J.C.G., Schenk, K.J., Piguet, C., Hopfgartner, G., (2001) Inorg. Chem., 40, p. 2642Terazzi, E., Torelli, S., Bernardinelli, G., Rivera, J., Benech, J., Bourgogne, C., Donnio, B., Piguet, C., (2005) J. Am. Chem. Soc., 127, p. 888Sarkar, D., Pramanik, A.K., Mondal, T.K., (2013) Spectrochim. Acta A-M, 115, p. 421Liu, Q.X., Wei, Q., Zhao, X.J., Wang, H., Li, S.J., Wang, X.G., (2013) Dalton Trans., 5902Wang, X.L., Hou, L.L., Zhang, J.W., Liu, G.C., Lin, H.Y., (2013) Polyhedron, 61, p. 65Kong, L., (2009) Acta Crystallogr., Sect. e, E65, p. 316Perumal, S., Mariappan, S., Selvaraj, S., (2004) Arkivoc, 8, pp. 46-51Hey, J.H., Zhi, Y.X., Zhi, Y.Z., Li, J., Zhang, F.X., (2013) J. Coord. Chem., 66, p. 1320(1997) Enraf-Nonius, , COLLECT Nonius BV Delft, The NetherlandsOtwinowski, Z., Minor, W., Denzo, H.K.L., (1997) Methods in Enzymology, 276, p. 307. , C.W. Carter Jr, R.M. Sweet (Eds) Academic Press, New YorkParkin, S., Moezzi, B., Hope, H., (1995) J. Appl. Cryst., 28, p. 53Sheldrick, G.M., (1997) SHELXS-97, Program for Crystal Structure Refinement, , University of Gottingen, GermanySheldrick, G.M., (1997) SHELXS-97, Program for Crystal Structure Analysis, , University of Gottingen, Germany(2005) TOPAS-R (Version 3.0), , Bruker AXS Karlswhe GermanyMota, V.Z., Carvalho, G.S.G., Corbi, P.P., Bergamini, F.R.G., Formiga, A.L.B., Diniz, R., Freitas, M.C.R., Da Cuin, A., (2012) Spectrochim. Acta A-M, 99, p. 110Roopashree, B., Gayathri, V., Mukund, H., (2012) J. Coord. Chem., 65, p. 1354Bowmaker, G.A., Fariati, E., Rahajoe, S.I., Skelton, B.W., White, A.H., (2011) Z. Anorg. Allg. Chem., 637, p. 1361Nilsson, K.B., Maliarik, M., Persson, I., Sandstrom, M., (2008) Dalton Trans., 2303Farrugia, L.J., (1997) J. Appl. Cryst., 30, p. 565Keller, E., (1986) Chem. Unserer Zeit, 20, p. 178Manjunatha, M.N., Dikundwar, A.G., Nagasundara, K.R., (2011) Polyhedron, 30, p. 1299Yang, H.W., Yue, F., Feng, S., Wang, J.D., Liu, H.A., Chen, H.M., Yu, K.B., Chin, Y.H., (2004) J. Org. Chem., 24, p. 792Xiao, B., Hou, H., Fany, Y., (2009) J. Coord. Chem., 62, p. 1827Hou, X.-Y., Wang, X., Fu, F., Wang, J.-J., Tang, L., (2013) J. Coord. Chem., 66, p. 3126Cui, Y., Yue, Y., Qian, G., Chen, B., (2012) Chem. Rev., 112, p. 112

Microwave-assisted multicomponent synthesis of julolidines using silica- supported calix[4]arene as heterogeneous catalyst

In this work, the multicomponent Povarov reaction was used for the synthesis of tetrahydrofuranjulolidines catalyzed by Si(n)CX[4]SO 3 H and assisted by microwave. The heterogeneous catalyst was synthesized from the p-sulfonic acid calix[4]arene by the sol-gel technique. The Povarov reaction is a multicomponent reaction between an aniline, analdehyde and an alkene or alkyne, catalyzed by Lewis or Brønsted acids, and can provide tetrahydroquinolines, quinolines or julolidines as products, depending on the reactive conditions employed. In this work, 24 julolidines were synthesized from different p-substituted anilines, formaldehyde and 2,3-dihydrofuran. The optimized conditions for the synthesis were: aniline (0.5 mmol), formaldehyde (1.5 mmol), 2,3-dihydrofuran (1.5 mmol), temperature of 150 °C,reaction time of 10 minutes, catalyst concentration of 0.5 mol%, in the absence of solvents. Yields ranged from 58 to 97%. The julolidines were obtained as a mixture of diastereoisomers, which were separated by a silica gel chromatography column, providing 12 julolidines with cis stereochemistry and 12 julolidines with (±)-trans stereochemistry. Compounds were identified and characterized by mass spectrometry, infrared spectroscopy, chiral column HPLC and 1 H and 13 C Nuclear Magnetic Resonance. The great advantage of the developed methodology is the short reaction time, the operational simplicity and the absence of solvents, factors that help to reduce the formationof residues and go according to the principles of green chemistry.Fil: de Paiva, Walysson F.. Universidade Federal de Vicosa; BrasilFil: Braga, Ingredy B. Universidade Federal de Vicosa; BrasilFil: de Assis, Joao V.. Universidade Federal de Vicosa; BrasilFil: Castañeda, Sandra M. B.. Universidade Federal de Vicosa; BrasilFil: Sathicq, Angel Gabriel. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - La Plata. Centro de Investigación y Desarrollo en Ciencias Aplicadas "Dr. Jorge J. Ronco". Universidad Nacional de la Plata. Facultad de Ciencias Exactas. Centro de Investigación y Desarrollo en Ciencias Aplicadas; ArgentinaFil: Palermo, Valeria. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - La Plata. Centro de Investigación y Desarrollo en Ciencias Aplicadas "Dr. Jorge J. Ronco". Universidad Nacional de la Plata. Facultad de Ciencias Exactas. Centro de Investigación y Desarrollo en Ciencias Aplicadas; ArgentinaFil: Romanelli, Gustavo Pablo. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - La Plata. Centro de Investigación y Desarrollo en Ciencias Aplicadas "Dr. Jorge J. Ronco". Universidad Nacional de la Plata. Facultad de Ciencias Exactas. Centro de Investigación y Desarrollo en Ciencias Aplicadas; ArgentinaFil: Natalino, Ricardo. Universidade Federal de Vicosa; BrasilFil: Martins, Felipe T.. Universidade Federal de Goiás; BrasilFil: de Carvalho, Gustavo S.G.. Universidade Federal de Juiz de Fora; BrasilFil: Amarante, Giovanni W.. Universidade Federal de Juiz de Fora; BrasilFil: Fernandes, Sergio A.. Universidade Federal de Vicosa; Brasil43ª Reunião Anual Virtual da SBQNo consignaBrasilSociedade Brasileira de Químic

Silver(I) complexes with symmetrical Schiff bases: Synthesis, structural characterization, DFT studies and antimycobacterial assays

Synthesis, structural and spectroscopic characterizations, molecular modeling and antimycobacterial assays of new silver(I) complexes with two Schiff bases - MBDA and MBDB - are reported. The complexes [Ag(MBDA) 2]NO3, or AgMBDA, and [Ag(MBDB)NO3] or AgMBDB, were obtained by the reaction of the respective ligands with silver(I) nitrate in methanol. The Schiff bases were previously obtained by mixing ethylenediamine or 1,3-diaminopropane with p-anisaldehyde. The characterizations of the complexes were based on elemental (C, H and N) and thermal (TG-DTA) analyses and 13C and 1H NMR and FT-IR spectroscopic measurements, as well as X-ray structure determination for AgMBDA. Spectroscopic data predicted by DFT calculations are in agreement with the experimental data for the AgMBDA complex. The AgMBDA complex has a monomeric structure with a molar proportion 1:2 Ag/ligand, while AgMBDB presents a 1:1 proportion. The complexes AgMBDA and AgMBDB showed to be more effective against Mycobacterium tuberculosis than antibacterial agent silver sulfadiazine - SSD. © 2013 Elsevier Ltd. All rights reserved

Initial invasive or conservative strategy for stable coronary disease

BACKGROUND Among patients with stable coronary disease and moderate or severe ischemia, whether clinical outcomes are better in those who receive an invasive intervention plus medical therapy than in those who receive medical therapy alone is uncertain. METHODS We randomly assigned 5179 patients with moderate or severe ischemia to an initial invasive strategy (angiography and revascularization when feasible) and medical therapy or to an initial conservative strategy of medical therapy alone and angiography if medical therapy failed. The primary outcome was a composite of death from cardiovascular causes, myocardial infarction, or hospitalization for unstable angina, heart failure, or resuscitated cardiac arrest. A key secondary outcome was death from cardiovascular causes or myocardial infarction. RESULTS Over a median of 3.2 years, 318 primary outcome events occurred in the invasive-strategy group and 352 occurred in the conservative-strategy group. At 6 months, the cumulative event rate was 5.3% in the invasive-strategy group and 3.4% in the conservative-strategy group (difference, 1.9 percentage points; 95% confidence interval [CI], 0.8 to 3.0); at 5 years, the cumulative event rate was 16.4% and 18.2%, respectively (difference, 121.8 percentage points; 95% CI, 124.7 to 1.0). Results were similar with respect to the key secondary outcome. The incidence of the primary outcome was sensitive to the definition of myocardial infarction; a secondary analysis yielded more procedural myocardial infarctions of uncertain clinical importance. There were 145 deaths in the invasive-strategy group and 144 deaths in the conservative-strategy group (hazard ratio, 1.05; 95% CI, 0.83 to 1.32). CONCLUSIONS Among patients with stable coronary disease and moderate or severe ischemia, we did not find evidence that an initial invasive strategy, as compared with an initial conservative strategy, reduced the risk of ischemic cardiovascular events or death from any cause over a median of 3.2 years. The trial findings were sensitive to the definition of myocardial infarction that was used