Synthesis,Crystal Structure and Biological Activity of 2-(1-(3-Bromo-1-(3-chloropyridin-2-yl)-1H-pyrazole-5-carbonyl)piperidin-4-yl)-N-isopropyl-1,3-thiazole-4-carboxamide

The title compound 2-(1-(3-bromo-1-(3-chloropyridin-2-yl)-1H-pyrazole-5-carbonyl)piperidin-4-yl)-N-isopropylthiazole-4-carboxamide(C21H22Br Cl N6O2 S,Mr = 536.04) has been synthesized,and its structure was characterized by IR spectra,1H-NMR,13C-NMR,EA,and single-crystal X-ray diffraction.The crystal of the title compound belongs to monoclinic system,space group P/c with a = 15.146(3),b = 11.573(2),c = 26.937(5) ?,β = 103.64(3)°,V = 1839.0(6) ?3,Z = 4,Dc = 1.557 g/cm3,μ(Mo Ka) = 0.71073 mm-1,F(000) = 2192,R = 0.0601 and w R = 0.1392.There exist one intramolecular hydrogen bond at N–H···N and four intermolecular weak interactions at O(2)···H(1),Cl(1)···H(12),O(1)···Cl(1) and S(1)···O(2).Bioassay results indicated that the title compound had good fungicidal and antiviral activities against tobacco mosaic virus.     

2, 2, 4, 13, 13, 15, —六甲基—1, 5, 12, 16—四氮杂环二十二烷—N′, N″′—二乙酸及其镧系配合物的合成和表征

本文合成了题头所示大环配体,并制备了它的十四种镧系元素(La～Lu,Pm除外)固体配合物.用元素分析,DTA-TG,红外光谱以及电导测定等手段研究了这些化合物的组成和性质.基于这些分析结果可建议配合物化学式为Ln(H₂L)(NO₃)₃·nH₂O.     

2,2,4,13,13,15,—六甲基—1,5,12,16—四氮杂环二十二烷—N′,N″′—二乙酸及其镧系配合物的合成和表征

本文合成了题头所示大环配体,并制备了它的十四种镧系元素(La～Lu,Pm除外)固体配合物。用元素分析,DTA-TG,红外光谱以及电导测定等手段研究了这些化合物的组成和性质.基于这些分析结果可建议配合物化学式为Ln(H_2L)(NO_3)_3·nH_2O。     

The Structure of Tris(3',5'-dimethylpyrazol-1-yl)-s-triazine and Its Use as a Ligand in Coordination Chemistry

The crystal and molecular structure of the title compound (Me₂-TPzT) has been determined by X-ray analysis. The observed molecular conformation presents the nitrogen atoms of three pyrazole rings in the same relative positions. The molecules are joined through intermolecular contacts forming chains that are arranged in a distorted hexagonal symmetry. Two complexes containing this ligand have been prepared: [{Pd(en)}₃(Me₂-TPzT)](PF₆)₆ and [{Ag(PPh₃)}3(Me₂-TPzT)](ClO₄)₃, which, due to their insolubility, have been characterized only by microanalysis, IR, ¹H NMR and, in the latter case, by mass spectrometry.     

新型吡唑并嘧啶并吡唑三元稠合化合物的合成

Novel fused heterotricyclic compounds 3—6 containing two different dipyrazolopyrimidine framework were prepared from 1a—1d. The reaction of 1 with K2CO3 in DMSO or NaH in DMF led to the formation of 2 or 3, respectively, which reacted further to afford 6 or 5, respectively.     

Cyclization of N-(2,4,6-trimethylphenyl)-β-alanines

Reaction of 2,4,6-trimethylaniline with acrylic and itaconic acids gives the corresponding N-substituted =alanines which can be converted to derivatives of tetrahydropyridone, dihydropyrimidinedione, and 4-carboxy-2-pyrrolidinone. Bromination of the aromatic substituent in the synthesized heterocycles has been carried out.Kaunas Technological University, Kaunas 3028, Lithuania Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 7, pp. 951–954, July, 2000     

Influence of inorganic anions on the tautomeric equilibria of N-substituted aminoazobenzenes — The evidence for ionic association

The influence of inorganic anions: perchlorate, chloride, sulphate, and hydrogen sulphate on the acid-base and tautomeric equilibria of 4-aminoazobenzene (AAB) and its N-ethyl (EAAB), N,N-diethyl (DEAAB), and N-phenyl (PhAAB) derivatives was investigated by UV-spectrophotometry in 80%:20% vol. ethanol:water system. The possible equilibrium models were evaluated by means of the nonlinear confluence analysis program STOICHIO in order to explain the observed dependence of the electronic spectra on acid and salt concentration. It was found that all the anions considered form 1:1 associates with both ammonium and azonium tautomers of the protonated aminoazobenzenes. The corresponding association constants were generally about one order of magnitude greater for SO ₄ ^2– than for the univalent ions. The azonium species were found to form more stable associates in all the cases except SO ₄ ^2– , which explains the observed shift of the tautomeric equilibrium towards the azonium form on increasing the mineral acid or salt concentration. Based on the obtained values of the molar absorption coefficients all but the PhAAB associates were found to be of the ionic pair type, with proton transfer taking place only in the last case. This was due to the greater basicity SO ₄ ^2– , compared with PhAAB. The association constant values obtained are discussed in terms of the tendency of the anions studied to associate, as well as in terms of the effect of solvation on the stability of the ionic pairs formed.     

Unusual reaction of N-aroyldihydrocyclopenta-pyrazolidinol with ketenes: formation of 1,3,4-oxadiazoles

1-Benzoyl-5-hydroxy-pyrazoline 1 was prepared and its reactions with ketenes, prepared in situ from the corresponding acid chlorides 3a-3d and the mixed anhydride 4, were studied. In all cases the 1,3,4-oxadiazoles 5 were isolated. In the case of compounds 3c and 3d a second diastereomeric oxadiazole 6 was obtained. In the case of 3a,3b and 4, an interesting aroyl migration product 7 was isolated. Structural assignments of the derived compounds were established by analysis of their IR, MS and NMR spectra (¹H, ¹³C, COSY, NOESY, HETCOR and COLOC). The proposed reaction mechanism is supported by semi-empirical (AM1) MO calculations.