Phosphor- und Schwefelhydrazin-Verbindungen / Phosphorus- and Sulfurhydrazine-Compounds

1971 ◽  
Vol 26 (12) ◽  
pp. 1232-1235 ◽  
Author(s):  
Herbert W. Roesky ◽  
Olaf Petersen

Pyrosulfonyldifluoride reacts with waterfree hydrazine in a molar ratio of 2 : 3 to give hydrazine -1,2-bis(sulfonylfluoride) in a low yield.. The reaction of N-fluorosulfonylamide and SOCl2 yields NH4⊕⊖ N(SO2F)2. This salt is converted to (C6H5)4P⊕⊖N(SO2F)2 in water by (C6H5)4PCl. (CH3)2NNH2 reacts with PSF3, PSF2Br, PSF2CH3 or PSF2C2H5 to yield the following compounds: (CH3)2NNHPSF2, (CH3)2NN (PSF2)2, (CH3)2NNHPSFCH3 and (CH3)2NNHPSFC2H5. The properties and the chemical behaviour of these substances are described. Results of ir-spectra, as well as 31P-, 19F- and 1H-nmr- and mass-spectra and elemental analysis characterize the compounds.

1971 ◽  
Vol 26 (7) ◽  
pp. 679-683 ◽  
Author(s):  
Herbert W. Roesky ◽  
Enno Janssen

P3N3F5NCO was prepared by reaction of P3N3F5NSO with (COCl) 2. Substituted amides were obtained from the reaction of P3N3F5NSO with carbonic acids e. g. P3N3F5NHCOCH3, P3N3F5NHCOC2H5, and P3N3F5NHCOC3H7. If these substances were treated with PCl5 the following compounds P3N3F5N = CClCH3, P3N3F5N = CClCH5, and P3N3F5TN = CClC3H7 were formed. They reacted with nucleophiles to give P3N3F5N = CNH2CH3, P3N3F5N = TN (CH3) 2C2H5, and P3N3F5N = CN (CH3) 2CH7. The properties of these compounds are described. They were characterized by elemental analysis and IR-spectra. 19F-, 1H-NMR, and mass spectra are reported.


2013 ◽  
Vol 2013 ◽  
pp. 1-14 ◽  
Author(s):  
Gauri D. Bajju ◽  
Sujata Kundan ◽  
Ashu Kapahi ◽  
Deepmala Gupta

Reaction of 5,10,15,20-meso-tetra(p-chlorophenyl)porphyrin[H2(p-Cl)pp] with zinc(II)acetate(Zn(OAc)2) and phenols results in the formation of corresponding axially ligated zinc(II)-meso-tetra(p-chlorophenyl)porphyrin (X-Zn-t(p-Cl)PP) (X = phenolates and pyridinates). The four-coordinated zinc porphyrin accepts one axial ligand in 1 : 1 molar ratio to form five-coordinated complex, which is purified by column chromatography and characterized by IR spectra,1H NMR, electronic absorption spectra, elemental analysis, mass spectroscopy, and TGA/DTA studies. IR spectra confirms the appearance of Zn– at 500–400 cm−1, Zn– at 650–570 cm−1and Zn–O at 650–350 cm−1.1H NMR spectra show that the protons of the Phenolic ring axially attached to the central metal ion are merged with the protons of the tetraphenyl rings of the porphyrin moiety. Absorption spectra reveal that complexes are accompanied by blue shift (hypsochromic shift) for phenolates and red shift (bathchromic shift) for pyridinates in comparison with the basic Zporphyrin emission bands. Mass Spectra determine them/zratio. The percentage of each element is confirmed by elemental analysis. According to the thermal studies, the complexes have a higher thermal stability and the decomposition temperature of these complexes depends on the axial ligation. Theinvitroantifungal activity of the complexes synthesized above had been done by disc diffusion method against the pathogen “Fusarium spp.,” which shows that with the increase in the concentration of the complexes, the colony diameter decreases and hence percent inhibition increases.


2013 ◽  
Vol 2013 ◽  
pp. 1-11 ◽  
Author(s):  
Lakhdar Sibous ◽  
Embarek Bentouhami ◽  
Mustayeen Ahmed Khan

4,4′-Diaminobiphenyl reacts with 2,4-pentanedione in absolute ethanol in a molar ratio 1 : 2 to form mainly the product of [1 + 2] condensation, 4,4′-(biphenyl-4,4′-diyldinitrilo)dipentan-2-one (H2L). The Schiff base was used as tetradentate chelating ligand to coordinate CoII and NiII chlorides leading to complexes where the ratio of metal ligand was found to be 2 : 1 or 2 : 2. All the synthesized products were characterized by elemental analysis, infrared, electronic, and mass spectroscopy, 1H NMR, and DSC. The electrochemical behaviour of the ligand and its complexes in DMF is also investigated.


2010 ◽  
Vol 75 (1) ◽  
pp. 105-119 ◽  
Author(s):  
Vojtech Varga ◽  
Jiří Pinkas ◽  
Róbert Gyepes ◽  
Petr Štěpnička ◽  
Michal Horáček ◽  
...  

Protocols for obtaining defined zirconocene complexes with polyhedral oligomeric silsesquioxanes with mono-, di-, and trisilanol functionality (SIPOSS, DIPOSS, and TRIPOSS) were established. The TRIPOSS silanolates binding one zirconocene and one chlorozirconocene moiety, [{(c-C5H9)7Si7O9O3}Zr2Cl(η5-C5H4R)4] (1, R = Bu; 2, R = H), were obtained by reacting the silanol with the respective zirconocene dichloride and triethylamine in CH2Cl2 in a 1.0:3.0:3.0 molar ratio, an excess of the zirconocene dichloride being required to suppress intramolecular dehydration of TRIPOSS. The related SIPOSS complex, [{(c-C5H9)7Si8O12O}2Zr(η5-C5H4Bu)2] (3), was prepared similarly at the stoichiometric ratio of [ZrCl2(η5-C5H4Bu)2]/ SIPOSS/NEt3 equal to 1.0:2.0:2.0. When employed in the 1.0:1.0:1.0 ratio, the same reagents afforded only the impure complex [{(c-C5H9)7Si8O12O}ZrCl(η5-C5H4Bu)2] (4), contaminated with 3 and unreacted [ZrCl2(η5-C5H4Bu)2]. Finally, the zirconocene complexes with SIPOSS and DIPOSS moiety, [{(c-C5H9)7Si8O12O}2Zr(η5-C5H5)2] (5) and [(c-C5H9)7Si7O9(OSiMe3)O2}- Zr(η5-C5H5)2] (6), respectively, were obtained by reacting [ZrMe2(η5-C5H5)2] with stoichiometric amounts of the appropriate silanols. All complexes were characterized by 1H, 13C, 29Si NMR and IR spectra, and by elemental analysis from XPS spectra. Preliminary ethene polymerization experiments showed that compounds 5 or 6 when combined with an excess of methylaluminoxane were nearly as active as [ZrCl2(η5-C5H5)2] whereas compound 2 was by about one order of magnitude less active.


RSC Advances ◽  
2017 ◽  
Vol 7 (24) ◽  
pp. 14389-14394 ◽  
Author(s):  
Ling-Bao Xing ◽  
Fei Qiao ◽  
Zhao Yuan ◽  
Jing-Li Zhang ◽  
Rui-Ying Zhang ◽  
...  

New binuclear alkynylplatinum(ii) terpyridyl complexes with flexible bridges have been synthesized and characterized by 1H NMR, mass spectra and elemental analysis.


2019 ◽  
Vol 31 (3) ◽  
pp. 613-616
Author(s):  
Vishwa Deepak Tripathi ◽  
Akhilesh Kumar Shukla ◽  
Hasan Shamran Mohammed

In present work, we have reported the synthesis and characterisation of novel hexahydrospiro[indoline-3,3′-pyrrolizine]-2-one derivatives in good to excellent yields via [3+2] cycloaddtion reaction in regioselective manner. These compounds were synthesized via multicomponent reaction of substituted 3-cinnamoyl-4-hydroxy-6-methyl-2H-pyran-2-one, isatin, L-proline at room temperature. All the synthesized hexahydrospiro molecules were characterized by 1H and 13C NMR, IR spectra, mass spectra and elemental analysis. Regioselectivity in synthesized molecules were also explained on the basis of secondary orbital interactions. A simple and facile methodology is developed which has great importance in synthetic chemistry.


2005 ◽  
Vol 09 (06) ◽  
pp. 430-435 ◽  
Author(s):  
Can-Cheng Guo ◽  
Tie-Gang Ren ◽  
Jian Wang ◽  
Chun-Yan Li ◽  
Jian-Xin Song

Five new meso-tetrakis(1-arylpyrazol-4-yl)porphyrins were synthesized to investigate their fluorescence properties. Preparation of these porphyrins was carried out by cyclization of tetramethoxypropane with substituted phenylhydrazine, followed by formylation to give the corresponding aldehydes, which reacted with pyrrole under the Adler reaction condition to get the target porphyrins (1a-1e). All the porphyrins were characterized by 1 H NMR, elemental analysis, UV-vis spectra and mass spectra. Red fluorescence emission of these porphyrins was observed in fluorescence spectra. Compared with meso-tetraphenylporphyrin (TPPH2), these meso-tetrakis(1-arylpyrazol-4-yl) porphyrins had a significant red shift in UV-vis and fluorescence spectra with increased fluorescence quantum yields.


2011 ◽  
Vol 322 ◽  
pp. 68-71
Author(s):  
Xi Shi Tai

Aβ-diketonate-type ligand, N-(3-methoxyl–phenyl)ketoacetamide (L), and its complexes with europium (III) and terbium (III) were synthesized. The ligand and complexes were characterized by elemental analysis, IR spectra,1HNMR spectra, mass spectra and luminescent spectra. The complexes were characterized by elemental analysis, IR spectra. The stoichiometry of metal-to-ligand in the complexes also was confirmed by the fluorescence behavior of the ligand and complexes in CH3CH2OH solution. In addition, the fluorescence properties of complexes in DMF, CH3OH, CH3CH2OH, acetone and CHCl3were investigated. The characteristic fluorescence of terbium (III) was assigned.


1971 ◽  
Vol 26 (2) ◽  
pp. 75-78 ◽  
Author(s):  
Herbert W. Roesky ◽  
Graalf Remmers

By reaction of N-sulfuroxideimides with phosphorus-pentabromide the compounds R-SO2NPBr3 (R = CH3 , CF3 , C6H5, p-Cl-C6H4, and p-CH3C6H4) were prepared. Reactions of hexamethyldisilazane and N- (dimethyl) -trimethylsilylamide resulted in the formation of R-SO2NPBr2N (CH3)2, (R = CH3, C6H5), and R-SO2NPBr2NHSi(CH3)3 (R = CF3, p-CH3-C6H4). The properties and the chemical behavior of these compounds are described. Results of IR-spectra, as well as 31P-, 19F-, and 1H-NMR-spectra and elemental analysis characterize the compounds.


2010 ◽  
Vol 7 (2) ◽  
pp. 545-550
Author(s):  
Kumar Sanjeev S. Lamani ◽  
Oblennavar Kortesh

A novel and efficient route have been designed for the synthesis of 4-(5-mercapto-1,3,4-thiadiazol-2-yl)-2-phenyl-5-[2-phenylvinyl]-2,4-dihydro-3H-1,2,4-triazol-3-one. All the synthesized compound were characterized by elemental analysis, IR,1H NMR,13C NMR and mass spectra. All the synthesized products were evaluated for their antibacterial activity againstB. SubtilisandE.Coliand antifungal activity againstA. nigerandC.Albicanrespectively. The results indicate that the present compounds may serve as better fungicides when compared to bactericides. The synthesized compounds have turned to be wonder by possessing antimicrobial properties.


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