Darstellung und Charakterisierung von einigen unsymmetrischen Chlordiorganophosphanen RR′PCI / Preparation and Characterization of Some Unsymmetrical Chlorodiorganophosphines RR′PCI

1989 ◽  
Vol 44 (4) ◽  
pp. 502-504 ◽  
Author(s):  
Jung Su Han ◽  
Werner Wolfsberger

Some unsymmetrical chlorophosphines RR′PCI were prepared by the reaction of RPCl2 (R = CH3, C2H5, i-C3H7, C6H5) with Grignard reagents R′MgCl (R′ = c-C5H9, c-C6H11, i-C3H7) and characterized by elemental analyses and spectroscopic data (IR, 31P and 13C NMR).

1991 ◽  
Vol 46 (11) ◽  
pp. 1578-1580 ◽  
Author(s):  
Werner Wolfsberger

Some (cyanomethyl)alkylphenyl phosphines R(C6H5)PCH2CN (R = CH3, C2H5, C3H7, C4H9, i-C4H9, C5H11,) were prepared by the reaction of the corresponding (trimethylsilyl)alkylphenyl phosphines with chloroacetonitrile and characterized by elemental analyses and spectroscopic data (IR; 1H, 31P and 13C NMR).


2007 ◽  
Vol 2 (11) ◽  
pp. 1934578X0700201 ◽  
Author(s):  
Katsumi Kusano ◽  
Tsukasa Iwashina ◽  
Junichi Kitajima ◽  
Tamaki Mishio

Nine Saussurea species, S. alberti, S. elegans, S. gnaphalodes, S. involucrata, S. konuroba, S. kuschakewiczii, S. leucophylla, S. schanginiana and S. sordida, and Serratula lyratifolia from the Tien Shan Mountains and adjacent area were chemically characterized for flavonoids. Thirty-one flavonoids and one hydroquinone were isolated from the leaves of these species and identified from mass spectrometric, UV, 1H and 13C NMR spectroscopic data, by characterization of hydrolyzates, and direct TLC and HPLC comparisons with authentic samples as kaempferol 3-O-rutinoside (1), quercetin 3-O-rutinoside (2), isorhamnetin 3-O-rutinoside (3), quercetin 3-O-glucoside (4), quercetin 3-O-galactoside (5), kaempferol 5-O-glucoside (6), kaempferol 7-O-glucoside (7), quercetin 5-O-glucoside (8), quercetin 7-O-glucoside (9), isorhamnetin 5-O-glucoside (10), luteolin (11), hispidulin (12), nepetin (13), selagin 7-methyl ether (14), selagin (15), velutin (16), luteolin 7-methyl ether (17), jaceosidin (18), apigenin 7-O-rutinoside (19), apigenin 7-O-glucoside (20), luteolin 7-O-rutinoside (21), luteolin 7-O-glucoside (22), luteolin 7-O-galactoside (23), luteolin 7-O-glucuronide (24), hispidulin 7-O-glucoside (25), nepetin 7-O-glucoside (26), luteolin 5-O-glucoside (27), isovitexin (28), apigenin 6,8-di-C-glycoside (29), isoorientin (30), luteolin 8-C-glycoside (31), and arbutin (32). The nine surveyed Saussurea species differed in their flavonoid composition. It was shown that the genus is not only morphologically, but also chemically diversified.


2015 ◽  
Vol 21 (5) ◽  
pp. 269-272 ◽  
Author(s):  
Snehal A. Chavan ◽  
Avinash G. Ulhe ◽  
Baliram N. Berad

AbstractNew 4,7-bis(arylamino)-2-tetra-O-acetyl-β-d-glucopyranosylimino-1,3,5,6-dithiadiazepines were synthesized via reaction of N-tetra-O-acetyl-β-d-glucopyranosyl isocyanodichloride with 1,6-diaryl-2,5-dithio-bis-ureas without using any catalyst. Thus, the synthesis of 7-membered heterocycles containing two sulfur and two nitrogen atoms through carbon-sulfur bond formation was explored. The chemical structures of these new compounds were elucidated by IR, 1H NMR, 13C NMR, mass spectral, and elemental analyses.


2003 ◽  
Vol 58 (12) ◽  
pp. 1165-1170 ◽  
Author(s):  
Sergey S. Karlov ◽  
Elmira Kh. Yakubova ◽  
Ekaterina V. Gauchenova ◽  
Anastasia A. Selina ◽  
Andrei V. Churakov ◽  
...  

The reaction of GeHal4 with MeN(CH2CH2OSiMe3)2 affords dihalogermocanes MeN(CH2 CH2O)2GeHal2 (1, Hal = Br; 2, Hal = Cl). Treatment of Me2Ge(NMe2)2 with MeN(CH2CH2OH)2 leads to dimethylgermocane MeN(CH2CH2O)2GeMe2 (3). The composition and structure of 1-3 were established by elemental analyses, 1H, 13C NMR spectroscopy, and mass spectrometry. The crystal structure of 1 is reported; structural data obtained from geometry DFT optimization on 1 are in good agreement with experimental results. Values of the electron density in the N→Ge bond critical point and the Laplacian of charge density for 1-3 indicate a closed-shell interaction between the Ge and N atoms.


1992 ◽  
Vol 70 (10) ◽  
pp. 2683-2687 ◽  
Author(s):  
Y. C. Toong ◽  
S. P. Tai ◽  
M. C. Pun ◽  
Rosemary C. Hynes ◽  
L. E. Khoo ◽  
...  

Methods of synthesis, elemental analyses, and IR and NMR spectroscopic data are reported for a series of triphenyltin esters of N-salicylidene-ω amino acids of the general formula: Ph3SnOCO(CH2)nN=CHAr (Ar = 2-HOC6H4− and 2-HOC10H6−; n = 1, 2, 3, and 5). The crystal structure of triphenyltin N-salicylidene-6-aminohexanoate was determined. The crystals are monoclinic, space group P21/a, with a = 16.3493(8) Å, b = 9.0675(7) Å, c = 18.8562(14) Å, β = 100.493(5)°, V = 2748.6(3) Å3, Z = 4, and Dcalc = 1.427 Mg m−3. The final discrepancy factors are RF = 0.033, and RW = 0.036 for 2339 significant reflections. This compound, believed typical of the series described, adopts a polymeric trans-O2SnC3 trigonal bipyramidal geometry with the axial positions occupied by a carboxylate oxygen and the phenolic oxygen of an adjacent molecule. These compounds appear to be the first reported triphenyltin(IV) carboxylates with phenolic oxygen bridges.


2021 ◽  
pp. 255-260 ◽  
Author(s):  
Shaban A. A. Abdel-Raheem ◽  
Adel M. Kamal El-Dean ◽  
Reda Hassanien ◽  
Mohamed E. A. El-Sayed ◽  
Mostafa Sayed ◽  
...  

Starting from 3-cyano-4,6-distyrylpyridin-2(1H)-thione (1), the compound N-(4-chlorophenyl)-2-((3-cyano-4,6-distyrylpyridin-2-yl)thio)acetamide (2) was prepared. Compound (2) underwent cyclization upon heating in ethanolic sodium ethoxide solution to give the corresponding cyclized form 3-amino-N-(4-chlorophenyl)-4,6-distyrylthieno[2,3-b]pyridine-2-carboxamide (3). The elemental analyses and spectroscopic data of compounds (2) and (3) are in agreement with their proposed structures. Their insecticidal activity against cowpea aphid, Aphis craccivora Koch, was studied. The results of insecticidal activity for compounds (2) and (3) against the nymphs and the adults of the tested insects exhibited that compounds (2) and (3) have a higher insecticidal activity than that of acetamiprid, a reference insecticide, after 24 h of treatment.


2007 ◽  
Vol 62 (11) ◽  
pp. 1353-1357 ◽  
Author(s):  
Aytaç Gürhan Gökçe ◽  
Rafet Kılınçarslan ◽  
Muhittin Aygün ◽  
Bekir Çetinkaya ◽  
Santiago García-Granda

A Pd(II) complex of a new N-heterocyclic carbene (NHC) ligand with bulky substituents and functionalized methoxy-donor side arms has been synthesized and characterized by elemental analyses, 1H and 13C NMR, and IR spectroscopy. Molecular and crystal structures of the title complex have been determined by single crystal X-ray diffraction. The compound crystallizes in the monoclinic space group P21/c, with a = 15.927(2), b = 8.489(2), c = 20.309(5) Å, β = 99.213(2)°, Z = 2, Dx = 1.253 g cm−3. The palladium atom is situated on an inversion center. There are several weak intramolecular C-H ··· N/O interactions.


2001 ◽  
Vol 56 (2) ◽  
pp. 137-140 ◽  
Author(s):  
Pavel L. Shutov ◽  
Sergey S. Karlov ◽  
Jörg Lorberth ◽  
Galina S. Zaitseva

Abstract Germanium, Azagermatranes The reaction of tris(dimethylamino)halogermanes, (Me2N)3GeHal (7, Hal = Cl; 8 , Hal = Br), with tris(2-aminoethyl)amines, N(CH2CH2NHR)3 (5, R = H; 6 , R = Me), yield l-halo-N,N',N"-azagermatranes (1, X = Cl, R = H; 2, X = Br, R = H; 3, X = Cl, R = Me; 4, X = Br, R = Me). Treatment of 4 with n-butyllithium affords l-n-butyl-N,N',N"-trimethylazagermatrane (14) in high yield. Reactions of n-BuLi with 7 or (Me2N)4Ge (13) lead to the formation of (Me2N)3Ge-n-Bu (15). On treatment of 15 with 5 the 1 -n-butylazagermatrane 16 was obtained. The molecular composition and the structures of all new compounds were established by elemental analyses, 1H and 13C NMR spectroscopy and mass spectrometry.


2019 ◽  
Vol 2019 ◽  
pp. 1-9
Author(s):  
Ibrahim A. M. Saraireh ◽  
Mohammednoor Altarawneh ◽  
Jibril Alhawarin ◽  
Mahmoud Salman ◽  
Abdel Aziz Abu-Yamin ◽  
...  

Schiff base diethyl 4,4-(pentane-2,4-diylidenebis(azanylylidene))benzoate (1) as a new ligand (L) was prepared by the reaction of acetylacetone with benzocaine in the ratio of 1 : 1. Two transition-metal complexes, [Ni(II)(LCl(HOEt))] (2) and [Zn(II)(LCl(HOEt))] (3), have been synthesized from metal salts with didentate Schiff base ligand (L) and characterized by elemental analyses, FT-IR, 1H NMR, 13C NMR UV-Vis spectroscopy, and magnetic susceptibility. The biological activity of the complexes was studied. In addition, the M06-2x density function theory method and the 6-31G(d) basic set were applied to determine the optimized structures of 1–3 and to determine their IR and 1H NMR, 13C NMR spectra theoretically. The data are in good agreement with the experimental results. The geometries of complexes 2 and 3 were determined to be square-planar for 2 and tetrahedral for 3.


1999 ◽  
Vol 54 (3) ◽  
pp. 363-371 ◽  
Author(s):  
Lothar Weber ◽  
Eckhard Dobbert ◽  
Andreas Rausch ◽  
Hans-Georg Stammler ◽  
Beate Neumann

The 2-halo-2,3-dihydro-1H-1,3,2-diazaboroles (1a′: R = tBu, X = Br; 1b: R = 2,6-Me2C6H3; X = I) were converted into the 2-amino-2,3-dihydro-1H-1,3,2- diazaboroles (2a: R = tBu; 2b: 2,6-Me2C6H3) by treatment with dry gaseous ammonia. Similarly reaction of 1a′ with 2,6-dimethylaniline or tBuNH2 afforded the corresponding derivates (3; R1 = 2,6-Me2C6H3; 4; R1 = tBu). The treatment of 1a′ with the ethylene diamine adduct of lithium acetylide led to the formation of (5). Lithiation of 2 a and subsequent silylation gave 6 (R1 = SiMe3), which was transformed to the diborolylamine (7) upon exposure to 1a′. Borolylketimine (8 ) and borolylcarbodiimide (9) resulted from 1a′ and Ph2C=NSiMe3 or Me3SiN=C=NSiMe3, respectively. All the new compounds were characterized by elemental analyses as well as spectroscopic data (IR, 1H, 11B, 13C NMR, MS). Heterocycle 5 was also subjected to an X-ray diffraction analysis.


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