共查询到20条相似文献,搜索用时 31 毫秒
1.
《Phosphorus, sulfur, and silicon and the related elements》2013,188(12):2659-2661
Manganese dioxide was found to catalyze stereoselective conversion of dialkyl 2-(imido-N-yl)-3-(triphenylphosphoranylidene)butanedioates to electron-poor (Z)-N-vinylimides in solvent-free conditions at 95°C in high coversions. 相似文献
2.
Ali Ramazani Abolfazl Momeni-Movahhed Farideh Gouranlou 《Phosphorus, sulfur, and silicon and the related elements》2013,188(4):903-907
Protonation of the highly reactive 1:1 intermediates, produced in the reaction between triphenylphosphine and dialkyl acetylenedicarboxylates, by 1-hydroxy-2-acetonaphthone leads to vinyltriphenylphosphonium salts, which undergo aromatic electrophilic substitution reaction with conjugate base to produce dialkyl 2-(3-acetyl-4-hydroxy-1-naphthyl)-3-(triphenylphosphoranylidene) butanedioates. Silica gel was found to catalyze conversion of dialkyl 2-(3-acetyl-4-hydroxy-1-naphthyl)-3-(triphenylphosphoranylidene) butanedioates to dialkyl 2-(3-acetyl-4-hydroxy-1-naphthyl)-2-butenedioates in solvent-free conditions at 90°;C in fairly good yields. 相似文献
3.
《Phosphorus, sulfur, and silicon and the related elements》2013,188(10):2189-2192
Protonation of the highly reactive 1:1 intermediates, produced in the reaction between triphenylphosphine and dialkyl acetylenedicarboxylates, by 1-hydroxy-2-acetonaphthone leads to vinyltriphenylphosphonium salts, which undergo aromatic electrophilic substitution reaction with conjugate base to produce dialkyl 2-(3-acetyl-4-hydroxy-1-naphthyl)-3-(triphenylphosphoranylidene) butanedioates. Microwave was found to catalyze conversion of dialkyl 2-(3-acetyl-4-hydroxy-1-naphthyl)-3-(triphenylphosphoranylidene) butanedioates to dialkyl 2-(3-acetyl-4-hydroxy-1-naphthyl)-2-butenedioates in the presence of silica gel powder in solvent-free conditions. 相似文献
4.
Shi-Wen Huang Jin-Sheng Cheng Li Qian Suo-Yi Huang 《Research on Chemical Intermediates》2011,37(1):1-9
Abstract
We present herein a new and efficient method for synthesis of bis-pyrazol pyrimidine derivatives by N-alkylation using a microwave-assisted synthetic process. Two new compounds, N-(4,6-bis(3,5-dimethyl-1H-pyrazol-1-yl)methyl nicotinonitrile and 2,6-bis(3,5-dimethyl-1H-pyrazol-1-yl)-4-methyl nicotinonitrile, were synthesized by the N-alkylation reaction. The novel compounds were characterized by Fourier transform infrared spectrometry, ultraviolet spectroscopy, elemental analysis, and nuclear magnetic resonance spectroscopy, etc. The microwave-assisted procedures have noteworthy advantages in terms of thermal efficiency over those carried out by conventional heating methods. 相似文献5.
《Phosphorus, sulfur, and silicon and the related elements》2013,188(10):2293-2295
Silica gel was found to catalyze the stereoselective conversion of dialkyl 2-(imido- N -yl)-3-(triphenylphosphoranylidene)butanedioates to electron-poor ( Z )- N -vinylimides in solvent-free conditions at 95°;C in high coversions. 相似文献
6.
R. I. Ishmetova N. I. Latosh I. N. Ganebnykh N. K. Ignatenko S. G. Tolshchina G. L. Rusinov 《Russian Journal of Organic Chemistry》2009,45(7):1102-1107
Reactions of 3,6-bis(4-R-3,5-dimethyl-1H-pyrazol-1-yl)-1,2,4,5-tetrazines and 3-amino-6-(3,5-dimethyl-1H-pyrazol-1-yl)-1,2,4,5-tetrazines with aliphatic alcohols and water in the presence of a base involved replacement of the dimethylpyrazolyl group and resulted in the formation of mono- and dialkoxy-1,2,4,5-tetrazines and 6-substituted 3-hydroxy-1,2,4,5-tetrazines. Dissociation constants of the latter were determined by potentiometric titration. 相似文献
7.
Ali Ramazani Ebrahim Ahmadi 《Phosphorus, sulfur, and silicon and the related elements》2013,188(7):1455-1457
Microwave was found to catalyze stereoselective conversion of dialkyl 2-(imido-N-yl)-3-(triphenylphosphoranylidene)butanedioates to electron-poor (Z)-N-vinylimides in the presence of iron(II) sulfate powder in solvent-free conditions in 4 min. 相似文献
8.
Two unexpected one-dimensional coordination polymers, [Cu(PT)(H2O)Cl]n 1 and [Cu2(BPT)(ClO4)3(H2O)4]n·2nH2O 2 , of symmetrical triazine-based ligands were synthesized by Cu(II)-mediated hydrolysis of the 2,4-bis(3,5-dimethyl-1H-pyrazol-1-yl)-6-methoxy-1,3,5-triazine ( MBPT ) pincer ligand. The reaction of Cu(ClO4)2·6H2O with MBPT proceeded via hydrolysis of the methoxy group to produce the dicompartmental 4,6-bis(3,5-dimethyl-1H-pyrazol-1-yl)-1,3,5-triazin-2(1H)-one ligand ( HBPT ) that then undergoes in situ complexation with Cu(II) to afford 2 . In case of CuCl2, the reaction proceeds further with C–N cleavage of one pyrazolyl unit leading to the formation of 6-(3,5-dimethyl-1H-pyrazol-1-yl)-1,3,5-triazine-2,4(1H,3H)-dione ligand ( HPT ) that also undergoes in situ complexation with Cu(II) affording 1 . The role of Cu(II) is to increase the Lewis acid reactivity of the water molecule where similar hydrolytic reactions for MBPT were observed in acidic medium in presence of an aqueous HCl (1:1 v/v) solution. The molecular and supramolecular structures of complexes 1 and 2 were investigated using X-ray diffraction of single crystal, Hirshfeld analysis, and density functional theory calculations. The Cl…H (11.7%) and O…H (24.7%) contacts are the most important in 1 , whereas the molecular packing of 2 is controlled mainly by the O…H (58.7%) hydrogen bonds. Complex 2 showed better activity against Escherichia coli, Bacillus subtilis, and Candida albicans compared with the standard antibiotics amoxicillin, tetracycline, and ampicillin. In general, complexes 1 and 2 showed good antimicrobial activity than these antibiotics and have the advantage to be used as both antibacterial and antifungal agents. 相似文献
9.
Ali Ramazani Ali Reza Kazemizadeh Farzin Marandi 《Phosphorus, sulfur, and silicon and the related elements》2013,188(7):1537-1540
Abstract Potassium dihydrogen phosphate powder and sodium dihydrogen phosphate powder were found to catalyze stereoselective conversion of dialkyl 2-(imido-N-yl)- 3-(triphenylphosphoranylidene)butanedioates to electron-poor (Z)-N-vinylimides in solvent-free conditions under microwave irradiation in 5-6 minutes in high conversions. 相似文献
10.
O. S. Attaryan S. K. Antanosyan G. A. Panosyan G. V. Asratyan S. G. Matsoyan 《Russian Journal of General Chemistry》2006,76(11):1817-1819
Formylation of N-alkyl-3,5-dimethyl-1H-pyrazoles according to Vilsmeier-Haak led to the formation of the corresponding 4-formyl derivatives. 3,5-Dimethyl-1H-pyrazole having no substituent on the nitrogen atom failed to undergo formylation at the 4 position under analogous conditions. 3,5-Dimethyl-1H-pyrazole-4-carbaldehyde was synthesized by alkaline hydrolysis of methyl β-(4-formyl-3,5-dimethyl-1H-pyrazol-1-yl)propionate and subsequent heating of the acid thus formed. 相似文献
11.
Avetisyan A. A. Aleksanyan I. L. Ambartsumyan L. P. 《Russian Journal of Organic Chemistry》2010,46(3):427-431
6(8)-Substituted 4-hydrazino-2-methylquinolines were synthesized by reaction of the corresponding 4-chloro-2-methylquinolines
with hydrazine hydrate. Reactions of the title compounds with ethyl acetoacetate and acetone gave 2,4-dimethyl-1H-pyrrolo[3,2-c]quinolines and 4-(5-ethoxy-3-methyl-1H-pyrazol-1-yl)-2-methylquinolines. 相似文献
12.
E. A. Nudnova A. S. Potapov A. I. Khlebnikov V. D. Ogorodnikov 《Russian Journal of Organic Chemistry》2007,43(11):1698-1702
New approaches have been proposed for the synthesis of compounds containing two bis(1H-pyrazol-1-yl)methane fragments. Nucleophilic replacement of the halogen atoms in appropriate tetrabromo derivatives by pyrazoles in the superbasic system KOH-DMSO gave ditopic chelating ligands: 1,1,2,2-tetrakis(1H-pyrazol-1-yl)ethane, 1,4-bis[bis(1H-pyrazol-1-yl)methyl]benzene, and 1,4-bis[bis(3,5-dimethyl-1H-pyrazol-1-yl)methyl]benzene. 1,4-Bis[bis(1H-pyrazol-1-yl)methyl]benzene was also synthesized by reaction of 1H-pyrazole with terephthalaldehyde in the presence of thionyl chloride. 1,1,2,2-Tetrakis(1H-pyrazol-1-yl)ethane was converted into the corresponding tetraiodo and tetranitro derivatives. 相似文献
13.
Synthesis of 4-Amino-3,5-dicyano-arylpyrazoles,Part 2: Isolation and Characterization of By-Products
M. S. T. Gonçalves A. M. F. Oliveira-Campos L. M. Rodrigues M. F. R. P. Proença 《合成通讯》2013,43(11):1695-1703
Reaction of (dicyanomethylidene-hydrazino)benzoic acids with chloroacetonitrile, under basic conditions, gave cyanomethyl-3-(7-amino-3,5-dicyano-1H-pyrazolo[4,3-d]pyrimidin-1-yl-benzoates and para-substituted cyanomethyl benzoates, in addition to the expected cyanomethyl 3-(4-amino-3,5-dicyano-1H-pyrazol-1-yl)-benzoates. 相似文献
14.
I. V. Taidakov B. E. Zaitsev A. N. Lobanov A. G. Vitukhnovskii N. P. Datskevich A. S. Selyukov 《Russian Journal of Inorganic Chemistry》2013,58(4):411-415
Neutral [EuL3Phen] complexes were synthesized by the reaction of EuCl3 with heterocyclic diketones-1-(1,5-dimethyl-1H-pyrazol-4-yl)-4,4,4-trifluoro-1,3-butanedione and 4,4,5,5,6,6,6-heptafluoro-1-(1-methyl-1H-pyrazol-4-yl)-1,3-hexanedione—and 1,10-phenanthroline (Phen) in an aqueous alcohol solution in the presence of NaOH. The reaction of GdCl3 with the same diketones under analogous conditions, but without adding 1,10-phenanthroline, yielded [GdL3(H2O)2] complexes. The composition of the complexes was determined by elemental analysis, and their optical and luminescent properties were examined. 相似文献
15.
In this study, we present the synthesis of 5-(3,5-dinitro-1H-pyrazol-4-yl)-1H-tetrazole and its energetic derivatives starting from 4-amino-3,5-dinitropyrazole, which was diazotized and cyanide substituted. A subsequent cycloaddition reaction with sodium azide led to 5-(3,5-dinitro-1H-pyrazol-4-yl)-1H-tetrazole ( 3 ). Several alkaline metal and nitrogen-rich salts were prepared and characterized by low-temperature X-ray diffraction. Additionally, all compounds were analyzed by vibrational spectroscopy (IR), 1H, 13C and 14N NMR spectroscopy, elemental analysis and differential thermal analysis (DTA). Additionally, the heats of formation for selected compounds were calculated using the atomization method based on CBS-4M enthalpies as well as important detonation parameters by using the EXPLO5 code (V6.05). Furthermore, the sensitivities of 3 and all synthesized salts toward friction, impact and electrostatic discharge according to BAM (Bundesamt für Materialforschung) were determined and compared to RDX. 相似文献
16.
L. V. Klyba L. K. Papernaya E. R. Sanzheeva A. A. Shatrova E. V. Rudyakova G. G. Levkovskaya 《Russian Journal of Organic Chemistry》2011,47(12):1851-1858
The mass spectra of 1-substituted 3,5-dimethyl-1H-pyrazole-4-carbaldehyde bis(2-hydroxyethyl) dithioacetals and thioacetals were studied for the first time. The main fragmentation
pathways of their molecular ions generated under electron impact and chemical ionization were similar. Primary decomposition
of the molecular ions of bis(2-hydroxyethyl) dithioacetals involves elimination of 2-sulfanylethanol molecule with formation
of the corresponding 1,3-oxathiolane radical cation. Fragmentation of the molecular ions [M]+ · and [M + H]+ derived from 2-(3,5-dimethyl-1H-pyrazol-4-yl)-1,4,6-oxadithiocanes includes cleavage of the eight-membered heteroring and elimination of C4H9OS ·. Substituents in the heteroring of pyrazolecarbaldehydes inhibit decomposition processes related to the aldehyde group. 相似文献
17.
Saied M. Soliman Hessa H. Al-Rasheed Jrg H. Albering Ayman El-Faham 《Molecules (Basel, Switzerland)》2020,25(23)
The self-assembly of iron(III) chloride with three pyrazolyl-s-triazine ligands, namely 2,4-bis(3,5-dimethyl-1H-pyrazol-1-yl)-6-(piperidin-1-yl)-1,3,5-triazine (PipBPT), 4-(4,6-bis(3,5-dimethyl-1H-pyrazol-1-yl)-1,3,5-triazin-2-yl)morpholine (MorphBPT), and 4,4’-(6-(3,5-dimethyl-1H-pyrazol-1-yl)-1,3,5-triazine-2,4-diyl)dimorpholine (bisMorphPT) afforded [Fe(PipBPT)Cl2][FeCl4] (1), [Fe(MorphBPT)Cl2][FeCl4] (2), and [H(bisMorphPT)][FeCl4]. bisMorphPT.2H2O (3), respectively, in good yield. In complexes 1 and 2, the Fe(III) is pentacoordinated with three Fe-N interactions from the pincer ligand and two coordinated chloride anions in the inner sphere, and FeCl4¯ in the outer sphere. Complex 3 is comprised of one protonated ligand as cationic part, one FeCl4¯ anion, and one neutral bisMorphPT molecule in addition to two crystallized water molecules. Analysis of molecular packing using Hirshfeld calculations indicated that H…H and Cl…H are the most important in the molecular packing. They comprised 40.1% and 37.4%, respectively in 1 and 32.4% and 37.8%, respectively in 2. Complex 1 exhibited the most bioactivity against the tested microbes while 3 had the lowest bioactivity. The bisMorphPT and MorphBPT were inactive towards the tested microbes while PipBPT was active. As a whole, the Fe(III) complexes have enhanced antibacterial and antifungal activities as compared to the free ligands. 相似文献
18.
V. M. Prokopenko S. G. Pil’o A. N. Vasilenko V. S. Brovarets 《Russian Journal of General Chemistry》2010,80(11):2358-2365
On the basis of methyl esters of 2-aryl-5-hydrazino-1,3-oxazole-4-carboxylic acids the earlier unknown methyl esters of 2-aryl-5-(3,5-dimethyl-1H-pyrazol-1-yl)-1,3-oxazole-4-carboxylic acids as well as their functional derivatives were synthesized. The latter were used
for further transformations, in particular, for introducing the residues of highly basic aliphatic amines into the 5 position
of oxazole, and the oxazol-2-yl moiety into the 4 position of the oxazole ring. 相似文献
19.
N. Missoum A. Guendouz N. Boussalah B. Hammouti A. Chetouani M. Taleb A. Aouniti S. Ghalem 《Research on Chemical Intermediates》2013,39(7):3441-3461
Methyl 2-(bis((3,5-dimethyl-1H-pyrazol-1-yl)methyl)amino) acetate, BT36, and methyl 2-(bis((3,5-dimethyl-1H-pyrazol-1-yl)methyl)amino)-3-(1H-indol-3-yl)propanoate, BT 43, have been synthesized. Investigation by weight-loss measurement and use of electrochemical techniques revealed the compounds are very effective inhibitors of corrosion of C38 steel in 1 M HCl solutions—percentage protection exceeded 95 % for BT43 at concentrations as low as 10?2 M. An impedance study in the absence and presence of these compounds revealed the mechanism of protection was cathodic inhibition by polarization and charge-transfer. The Langmuir adsorption isotherm was obeyed. Quantum chemical data calculated by use of DFT at the B3LYP/6-31G* level of theory revealed a good correlation between inhibition efficiency and the molecular structure of BT36 and BT43. The highest occupied molecular orbital, the lowest unoccupied molecular orbital, the separation energy (ΔE), and the dipole moment (μ) from the inhibitor to the metal surface explain the experimental data well. 相似文献
20.
Ş. Hakan Üngören Mustafa Saçmacı Cengiz Arıcı Ertan Şahin Taner Arslan Fatma Kandemirli 《Phosphorus, sulfur, and silicon and the related elements》2013,188(11):2877-2890
Novel alkyl substituted 3-(4-benzoyl-1,5-diphenyl-2,3-dihydro-1H-pyrazol-3-yl)-3-oxo-2-(triphenylphosphoranylidene) propanoates (3) were synthesized from 4-benzoyl-1,5-diphenyl-1H-pyrazole-3-carbonylchloride (1) and alkyl (triphenylphosphoranylidene) acetates (2a–b). The synthesized compounds were characterized by elemental analysis, spectroscopic studies (3a–b), and single crystal X-ray diffraction (3a). The mechanism of the reaction between (1) and (2a) was studied by AM1, and the geometrical parameters of the studied molecules were also carried out in B3LYP methods with the standard 6–31G (d,p) basis set. NBO analysis were studied for 1 and 2a B3LYP methods with the standard 6–31G (d,p) basis set. 相似文献