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1.
M. A. M. Khouna M. T. Ben Dhia M. R. Khaddar 《Phosphorus, sulfur, and silicon and the related elements》2013,188(7):1673-1682
The two octahedral complexes SnCl4·2(O)PF(NR2)2 (R = Me or Et) were prepared from reaction of SnCl4 with the ligand (R2N)2P(O)F in anhydrous CHCl3. The new adducts have been characterized by elemental analysis, IR, and multinuclear (119Sn, 31P, 19F, and 1H) NMR spectroscopy. The NMR data show that the adducts exist in solution as a mixture of cis and trans isomers with markedly different proportions. When compared with previously described hexamethylphosphoramide (HMPA) and trimethylphosphate (TMPA) analogues, our results indicate that the cis isomer is the predominant species in solution. Low temperature 31P and 119Sn NMR spectra show that the compounds partially dissociate in dichloromethane. 相似文献
2.
M. T. Ben Dhia M. A. M. K. Sanhoury C. Zenati M. R. Khaddar 《Phosphorus, sulfur, and silicon and the related elements》2013,188(11):3082-3089
The complexes CdL4(ClO4)2 (1), CdL2(NO3)2 (2), and CdL2Cl2 (3) (L = (Me2N)3P(Se)) have been prepared and characterized by elemental analysis, conductivity measurements, IR, and multinuclear (31P, 77Se, and 113Cd) NMR spectroscopy. 31P and 77Se NMR data were informative of changes associated with complex formation. The structure of the prepared complexes was further confirmed in solution by their 113Cd NMR spectra, which show a quintuplet for the perchlorate complex and a triplet for each of the nitrate and chloride complexes due, respectively, to coupling with four and two equivalent phosphorus atoms, consistent with a four coordinate tetrahedral geometry for the cadmium center. The NMR data are discussed and compared with those reported for related complexes. 相似文献
3.
M. T. Ben Dhia M. A. K. Sanhoury K. Essalah M. R. Khaddar 《Phosphorus, sulfur, and silicon and the related elements》2013,188(9):1922-1931
Abstract Four octahedral complexes of the type SnCl4.2L [L = (R2N)3P(E): E = Se; R = Me(1), Et(2) and E = S; R = Me(3), Et(4)] have been studied in solution by multinuclear (31P, 77Se, and 119Sn) NMR spectroscopy. 31P and 77Se NMR data were informative of changes associated with complex formation. The solution structure of the complexes was confirmed by their 119Sn NMR spectra that showed two triplet features for each complex, attributed to a mixture of the expected cis and trans isomers. The triplet signal is due to the coupling with two equivalent phosphorus atoms, consistent with an octahedral geometry around the tin center. In addition, density functional theory (DFT)/B3LYP calculations have been carried out to support the interpretations of NMR data. The results are discussed and compared with those reported for related complexes. GRAPHICAL ABSTRACT 相似文献
4.
Jochen Krill Igor V. Shevchenko Axel Fischer Peter G. Jones Reinhard Schmutzler 《Phosphorus, sulfur, and silicon and the related elements》2013,188(6):1217-1239
The reaction of the title compound 1 with the p-R-aniline derivatives (R═H, F, OCH3, NO2, and NH2) led to the formation of the aza-2σ3,4σ3-diphosphetidines 2a– 2e, whereas 2-trimethylsiloxyaniline furnished the azadiphosphetidine 2f. The reaction of the sterically crowded 2,6-dimethylaniline with 1 furnished the disubstituted derivative 3. The tricyclic compound 5 was formed during the reaction of 1,2-phenylenediamine with 1. Heptamethyldisilazane formed the aza-2σ 3 ,4σ 3 -diphosphetidine 6 on reaction with 1. The bulkier tert.-butylamine formed with 1 a mixture of the aza-2,4-diphosphetidine 7a and the disubstituted derivative 7b, which could not be separated. The reaction of 2b and 6 with tetrachloro-o-benzoquinone resulted in the formation of the bis-spirophosphoranes 8 and 9b, respectively. The formation of the monospirophosphorane 9a was observed in the 31P NMR spectrum. The characterization of compounds is based in particular on NMR investigations (1H, 13C, 31P). 2a was characterized by a single-crystal X-ray structure analysis. The dimethylurea fragment is planar; the four-membered ring is folded about the P···P vector by 38.7°. 相似文献
5.
Thouraya Barhoumi-Slimi M. A. K. Sanhoury M. T. Ben Dhia M. R. Khaddar 《Phosphorus, sulfur, and silicon and the related elements》2013,188(9):1220-1227
Abstract The reaction of SnCl4 with β-chlorovinyl aldehydes in anhydrous dichloromethane gave a series of octahedral complexes of the general formula SnCl4·2L (L = aldehyde). The adducts have been characterized in solution using multinuclear (1H, 13C, and 119Sn) NMR and IR spectroscopy. Solution NMR studies show that the complexes undergo rapid ligand dissociation at ambient temperature. Ligand exchange is slowed significantly at low temperature, such that, in most of the complexes, it is possible to identify both the cis and trans isomers with predominance of the cis form. The magnitude of the metal-ligand interaction was estimated on the basis of 119Sn NMR chemical shifts and used to classify the aldehydes studied according to their Lewis basicity. 相似文献
6.
R. I. Dzhalmakhanbetova S. A. Ivasenko A. T. Kulyyasov B. B. Khasenov N. B. Kurmankulov S. M. Adekenov 《Chemistry of Natural Compounds》2004,40(4):381-386
New phosphorus-containing derivatives of grosshemin were synthesized in 68-70% yield by reacting this guaianolide with dialkylphosphites. Their structures were established by IR, PMR, 13C NMR, and 31P NMR spectroscopies and two-dimensional 1H-1H NMR spectroscopy (COSY). The reaction of grosshemin with dialkylphosphites was found to be highly stereoselective. 相似文献
7.
R. I. Dzhalmakhanbetova E. M. Suleimenov B. B. Rakhimova N. A. Talzhanov A. T. Kulyyasov S. M. Adekenov 《Chemistry of Natural Compounds》2002,38(6):553-556
Novel dialkylphosphonates of arteannuin B were synthesized in 45-47% yields by reaction of this cadinanolide with dialkylphosphites. Their structures were established using IR, PMR, 13C and 31P NMR spectroscopy, and two-dimensional 1H-1H NMR (COSY) spectroscopy. The reaction of arteannuin B and dialkylphosphites is highly stereoselective. 相似文献
8.
Zdzisław Głowacki Maria Hoffmann 《Phosphorus, sulfur, and silicon and the related elements》2013,188(1-2):171-175
Abstract 31P chemical shifts are reported for 24 different models of diastereoisomeric phosphonodidepsipeptides coupled from the N-protected L-aminoacids and dibenzyl esters of chiral 1-hydroxyalkylphosphonic acids. The 31P NMR nonequivalence variations with the changing of didepsipeptide structure, solvent and temperature were investigated. Amide cis-trans isomerism were observed in the case of Z-L-proline derived didepsipeptides. 相似文献
9.
Poola Sreelakshmi Sarva Santhisudha Gajjala Raghavendra Reddy Yakkate Subbarao Kotha Peddanna Chippada Apparao 《合成通讯》2018,48(10):1148-1163
A new green and efficient method has been developed for the synthesis of α-aminophosphonates through one-pot three-component Kabachnik–Fields reaction. It involves the reaction of a 2-aminophenol with different substituted aromatic aldehydes and dimethyl phosphite in the presence of nanocopper oxide–gold (CuO–Au) catalyst under solvent-free conditions at 60?°C. Nano-CuO–Au catalyst was found to have many advantages like high activity, simple workup, and good (87%) to very high yields (96%). The products were characterized by IR, 1H, 13C, and 31P NMR spectra and elemental analysis. All the synthesized compounds were screened for in vitro antioxidant and α-glucosidase inhibition activities. The compound 4b showed higher 2,2-diphenyl-1-picrylhydrazyl and H2O2 radical scavenging activity and compound 4e showed higher NO radical scavenging activity than the standard ascorbic acid. The compound 4j has much higher α-glucosidase enzyme inhibition activity than the standard acarbose. 相似文献
10.
M. H. A. Elgamal N. M. M. Shalaby M. A. Shaban H. Duddeck B. Mikhova A. Simon G. Tóth 《Monatshefte für Chemie / Chemical Monthly》1997,128(6-7):701-712
Summary The synthesis of some dimeric coumarin and furanocoumarin models and their structure elucidation by1H NMR,13C NMR, and mass spectroscopy is presented. In the presence of moisture some aldehydes are accompanied by their hydrates. Methoxy signal doubling in the presence of a chiral lanthanide shift reagent proves the dimeric nature of compound8. In the mass spectra, heterolytic cleavage of the O-C linkage was noticed which is a rare fragmentation in the case of aromatic ethers.
Synthese und spektroskopische Untersuchung einiger dimerer Cumarin- und Furanocumarinmodelle
Zusammenfassung Die Synthese einiger dimerer Cumarin- und Furanocumarin-Modellverbindungen und ihre Strukturaufklärung mit1H- und13C-NMR- sowie Massenspektrometrie werden beschrieben. In Gegenwart von Feuchtigkeit werden einige der Aldehyde von ihren Hydraten begleitet. Verdoppelungen der Methoxy-1H-Signale von8 in Anwesenheit eines chiralen Lanthanoid-Verschiebungsreagenzes beweisen, daß8 ein Dimer ist. In den Massenspektren finden sich Hinweise für heterolytische Spaltungen der O-C-Bindungen. Solche Fragmentierungen sind bei aromatischen Ethern ungewöhnlich.相似文献
11.
A complex mixture of fluoro-polyphosphates (FPPs) and polyphosphates was prepared by heating a mixture of NaF and sodium tripolyphosphate (STPP) at 600 °C in nitrogen atmosphere. Two-dimensional 31P-19F heteronuclear correlation spectroscopy (HETCOR) NMR was developed in identifying the atomic connection between F and P in the mixed FPPs. 19F, 31P and 31P-31P correlation spectroscopy (COSY) NMR methods were employed to identify the components of the mixture and measure the chain length of each FPP ingredient. NMR results clearly demonstrated that the mixture contains four kinds of fluoro-phosphates with different chain length of polyphosphate, which are monofluoro-phosphate (MFP), monofluoro-dipolyphosphate (MFDPP), monofluoro-tripolyphosphate (MFTPP) and difluoro-tripolyphosphate (DFTPP). Other phosphates and polyphosphates also were found in the mixture. 相似文献
12.
T. Meier M. Braun W. Frank 《Phosphorus, sulfur, and silicon and the related elements》2013,188(10):2536-2544
The reaction of (S)-1,1,2-triphenylethanediol (3) with phosphorus trichloride leads to the diastereoselective formation of (S C,R P)-2-chloro-1,3,2-dioxaphospholane (2). Its configuration has been determined by single crystal X-ray diffraction. When reacted with racemic secondary alcohols, diastereomeric phosphites are obtained, which display substantial shift differences in the 31P NMR spectra. Thus, chlorodioxaphospholane 2 can serve as derivatizing reagent for chiral secondary alcohols permitting to determine their enantiomeric excess. 相似文献
13.
Synthesis of novel bis-(3-methyl-5-nitro-2-oxo-2,3-dihydro-2λ 5benzo[1,3,2]oxazaphosphol-2yl)substituted aryl methanes was accomplished by Pudovik reaction. Addition of equimolar quantities of 2-methylamino-4-nitro phenol (1) and ethanol to PCl3 afforded cyclic condensation product. On reaction with respective aldehydes followed by treatment with phosphorus(III) monochloride of 1, and on subsequent reaction at reflux temperature, this rearranged from P(III) to P(V) state. Their structures were determined by IR, 1H NMR, 13C NMR, 31P NMR, and mass spectral data. 相似文献
14.
Zied Hassen Bechir Hajjem 《Phosphorus, sulfur, and silicon and the related elements》2013,188(5):987-993
In the present work, we study the reaction of fluorinated hydrazines H 2 N-NHR F with α-ketophosphonates 1, which lead to N-fluoroalkylated α-phosphonylated hydrazones 2. The stereochemistry of the hydrazones 2 was determined by multinuclear NMR experiments ( 1 H, 13 C, 19 F, and 31 P) and IR spectroscopy. 相似文献
15.
A three-component reaction between 5,5-dimethylcyclohexan-1,3-dione (dimedone), aromatic aldehydes, and acetonitrile in the presence of chlorosulfonic acid afforded N-[(2-hydroxy-4,4-dimethyl-6-oxocyclohexene-1-yl)-aryl-methyl]-acetamides in good yields. The temperature-dependent 1H NMR of one of the products has been investigated. 相似文献
16.
The reaction of mercury(II) chloride with neutral phosphine telluride ligands (R3PTe) produced new mercury(II) complexes, HgCl2(R3PTe)2 [R = Me2N (1), Et2N (2), C4H8N (3), C5H10N (4) or n-Bu (5)]. Attempts to isolate the complex of HgCl2 with the morpholinyl ligand, (OC4H8N)3PTe, were unsuccessful. Complexes 1–5 have been characterized by elemental analyses, IR, and multinuclear (31P, 125Te, and 199Hg) NMR spectroscopy. The solution behavior of the complexes was investigated using variable temperature NMR spectroscopy in the presence of excess ligand and indicated fast ligand exchange on the NMR timescale at room temperature. The metal–ligand exchange barriers in these complexes were estimated to be in the range 8–11 kcal/mol. The results suggest that a slight change in the nature of the substituents on the phosphorus of the ligand can contribute considerably to the lability of the complex obtained. The NMR data are discussed and compared with those obtained for related phosphine chalcogenide systems. 相似文献
17.
Akbar Mobinikhaledi Hassan Moghanian Maryam Deinavizadeh 《Comptes Rendus Chimie》2013,16(11):1035-1041
A simple and efficient procedure for the synthesis of 9H-xanthene or bisphenol derivatives has been developed by one-pot condensation of xylenols with aromatic aldehydes in the presence of p-toluenesulfonic acid (pTSA) as a catalyst under solvent-free conditions at 100 °C. It is noteworthy that the condensation reaction of 3,5-xylenol with aldehydes produces 9H-xanthene derivatives, while the reaction with other xylenols leads to the corresponding bisphenol derivatives. Different types of aromatic aldehydes are used in the reaction and in every case the products were obtained in good to excellent yields. The structures of these compounds were established on the basis of IR, 1H NMR, 13C NMR and CHN data. 相似文献
18.
R. I. Dzhalmakhanbetova B. B. Rakhimova N. A. Talzhanov G. K. Rustembekova A. T. Kulyyasov S. M. Adekenov 《Chemistry of Natural Compounds》2002,38(6):549-552
Novel isoalantolactone dialkylphosphonates were synthesized in 70-87% yields by reacting this eudesmanolide with dialkylphosphites. Their structures were proved by spectral analysis using IR, PMR, 13C and 31P NMR, and two-dimensional 1H-1H (COSY) spectroscopy. The reaction of isoalantolactone with dialkylphosphites is highly stereoselective. 相似文献
19.
《Journal of Coordination Chemistry》2012,65(7):1107-1117
The reaction of [Rh(CO)2(µ-Cl)]2 with two molar equivalents of a chiral ligand, (R)-N,N-bis(2-diphenylphosphinoethyl)-1-phenylethylamine(PNP*) yield a mono-carbonyl complex, [Rh(CO)Cl(η2-P,P-PNP*)] (1), in which the potentially tridentate PNP* ligand coordinates in a bidentate fashion through P,P bonding. The complex was characterized by elemental analysis, FAB mass, IR, UV-Vis, 1H- and 31P{1H}-NMR spectroscopy. Variable temperature (223–298 K) 31P{1H}-,NMR spectra of 1 showed a mixture of cis and trans isomers in the solution with the trans predominating at room temperature and the cis at lower temperature. Complex 1 was immobilized on silica through axial coordination of amine from 3-aminopropyltriethoxysilane functionalized silica. The immobilized materials were characterized by elemental analysis (N2), FTIR, DTA–TGA, N2-adsorption, XRD, and SEM analysis. 相似文献
20.
PN Bond Cleavage during the Insertion of Carbon Fragments into PIIIN Bonds in Bis(diphenylphosphino) Amines
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The reaction of tertiary amine functionalized phosphines with aromatic and aliphatic aldehydes gives insertion of carbon fragments into the PIII? N bonds or PIII? N bond cleavage. The reaction of bis(diphenylphosphino) amines, 1a – 1c , with two equiv. of aldehydes in toluene afforded the PIII? N bond inserted products, 2a – 4a, 4b – 6b , and 3c – 5c , in moderate‐to‐good yield. The products were characterized by IR, 1H‐ and 31P‐NMR spectroscopy and elemental analysis. 相似文献