Syntheses and Characterization of 1-Haloazagermatranes

2001 ◽  
Vol 56 (2) ◽  
pp. 137-140 ◽  
Author(s):  
Pavel L. Shutov ◽  
Sergey S. Karlov ◽  
Jörg Lorberth ◽  
Galina S. Zaitseva
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Molecular Composition ◽  
High Yield ◽  
Elemental Analyses ◽  
New Compounds ◽  
C Nmr

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.

Synthesis and Characterization of 1-Allyl-3,7,10-trimethylgermatrane and 1-Allylazagermatranes

1998 ◽  
Vol 53 (11) ◽  
pp. 1255-1258 ◽  
Author(s):  
Galina S. Zaitseva ◽  
Bettina A. Siggelkow ◽  
Sergey S. Karlov ◽  
Gleb V. Pen’kovoy ◽  
Jörg Lorberth
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Synthesis And Characterization ◽  
Elemental Analyses ◽  
New Compounds ◽  
C Nmr

The reaction between Br3GeAll (1) and N(CH2CHMeOSnBu3)3 (2, mixture of isomers) yielded N(CH2CHMeO)3GeAll (3) as a mixture of diastereomers. Three azagermatranes of the type N(CH2CH2NR)3GeAll (9, R = H; 10, R = Me; 11, R = Me3Si) have been synthesized from the reaction of (Me2N)3GeAll (5) with N (CH2CH2NHR)3 (R = H, 6; Me, 7; Me3Si, 8). Composition and structures of the new compounds were established by elemental analyses, 1H and 13C NMR spectroscopy and mass spectrometry.

Synthesis and Crystal Structure of the Germatrane E-N(CH)2CH2O3GeC(Br)=C(Br)Ph

2003 ◽  
Vol 58 (7) ◽  
pp. 613-619 ◽  
Author(s):  
Anastasia A. Selina ◽  
Sergey S. Karlova ◽  
Klaus Harms ◽  
Daniil A. Tyurina ◽  
Yuri F. Oprunenko ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Nmr Spectroscopy ◽  
Dft Calculations ◽  
Molecular Composition ◽  
High Yield ◽  
Synthesis And Crystal Structure ◽  
Elemental Analyses ◽  
New Compounds ◽  
C Nmr

The reaction of (phenylacetylenyl)triethoxygermane, (EtO)3GeC≡CPh (3), with bromine in CHCl3/CCl4 solution leads to a mixture of Z- and E- (EtO)3GeC(Br)=C(Br)Ph (4) in the ratio Z/E = 3/1. Treatment of this product with N(CH2CH2OH)3 affords a mixture of Z- and EN(CH2CH2O)3GeC(Br)=C(Br)Ph (2) in high yield. Compound E-2 was isolated in 16% yield. The molecular composition and the structure of all new compounds have been established by elemental analyses, 1H and 13C NMR spectroscopy. The crystal structure of E-2 is reported. The possible reasons for the different Z/E ratios in the products of the bromination of 3 and N(CH2CH2O)3GeC≡CPh (1) are discussed using DFT calculations.

Synthesis and Structural Characterization of Metal Complexes of 2-Formylpyrrole 4N-Methylthiosemicarbazone (4ML1) and 2-Acetyl- pyrrole 4N-Methylthiosemicarbazone (4ML2). The X-Ray Crystal Structures of [Ni(4ML1-H)2], [Pd(4ML1-H)2] and [Cd(4ML2)2I2]

2001 ◽  
Vol 56 (3) ◽  
pp. 219-228 ◽  
Author(s):  
Ruben Alonso ◽  
Elena Bermejo ◽  
Rosa Carballo ◽  
Alfonso astiñeiras ◽  
Teresa Pérez
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Elemental Analysis ◽  
Structural Characterization ◽  
X Ray ◽  
Group 12 ◽  
New Compounds ◽  
Group 10 Metals ◽  
C Nmr

Abstract Reaction of 4N-methyl-2-[1-(pyrrol-2-yl)methylidene]hydrazinecarbothioamide (4ML1 and 4N-methyl-2-[1-(pyrrol-2-yl)-ethylidene]hydrazine carbothioamide (4ML1) with zinc(II), cadmium(II) and mercury(II) halides afforded complexes with formulas [M(L)X2] [(L; M; X) =(4ML1; Cd; Cl) (4), (4ML1; Hg; Cl, Br, I) (7 - 9), (4ML2; Cd; Cl) (17), (4ML2; Hg; Cl, Br, I) (20 - 22)] or [M(L)2X2] [(L; M; X) = (4ML1; Zn; Cl, Br, I) (1 - 3), (4ML1; Cd; Br, I) (5, 6), (4ML2; Zn; Cl, Br, I) (14 - 16), (4ML2; Cd; Br, I) (18, 19)]. Reaction of 4ML1 with salts of copper(II), nickel(II), palladium(II) and platinum(II) afforded complexes of formula [M(4ML1-H)2] (10 -13). Crystals of 11, 12 and 19 were studied by X-ray diffractometry, and all new compounds were characterized by elemental analysis, mass spectrometry, and IR, electronic and 1H and 13C NMR spectroscopy and, when pertinent and allowed by the solubility of the compound, 113Cd or 199Hg NMR spectroscopy. In the complexes of Group 12 metals, both ligands are neutral and S-monodentate. In the complexes of copper or Group 10 metals, 4ML1 is monodeprotonated and S,N-bidentate.

N-alkyl-2-(1,2-diferrocenylvinyl)-4,5-dihydrooxazolinium salts, multi-component synthesis and breaking of their heterocyclic systems

2016 ◽  
Vol 88 (12) ◽  
pp. 1129-1142 ◽  
Author(s):  
Jessica J. Sánchez García ◽  
Marcos Flores-Alamo ◽  
Mark E. Martínez Klimov ◽  
Elena I. Klimova
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Elemental Analysis ◽  
X Ray Diffraction ◽  
X Ray ◽  
Alkyl Iodides ◽  
New Compounds ◽  
C Nmr

AbstractA new multicomponent method for the synthesis of N-alkyl-2-(Z-1,2-diferrocenylvinyl)-4,5-dihydrooxazolinium salts 3a–f, 5-(N-alkyl-2′,3′-diferrocenyl-acryloylamido)-3-aza-3-alkylpentanols 4a–d, (E)-N-alkyl-N-(2-morpholinoethyl)-2,3-diferrocenylacrylamides 9a,b,e,f and (E)-N-alkyl-N-(2-piperidinoethyl)-2,3-diferrocenylacrylamides 10a,c from reactions of 2,3-diferrocenylcyclopropenone 1 with bis-1,4-N,O-nucleophiles in the presence of triethyloxonium tetrafluoroborate, alkyl iodides, morpholine, piperidine and Et3N is described. The characterization of the new compounds was done by IR, 1H- and 13C-NMR spectroscopy, mass-spectrometry, elemental analysis and X-ray diffraction studies.

scholarly journals Synthesis, characterization and DNA interaction studies of new triptycene derivatives

2014 ◽  
Vol 10 ◽  
pp. 1290-1298 ◽  
Author(s):  
Sourav Chakraborty ◽  
Snehasish Mondal ◽  
Rina Kumari ◽  
Sourav Bhowmick ◽  
Prolay Das ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Conformational Changes ◽  
Dna Interaction ◽  
High Yield ◽  
Efficient Synthesis ◽  
Elemental Analyses ◽  
Multinuclear Nmr Spectroscopy ◽  
Propiolic Acid

A facile and efficient synthesis of a new series of triptycene-based tripods is being reported. Using 2,6,14- or 2,7,14-triaminotriptycenes as synthons, the corresponding triazidotriptycenes were prepared in high yield. Additionally, we report the transformation of 2,6,14- or 2,7,14-triaminotriptycenes to the corresponding ethynyl-substituted triptycenes via their tribromo derivatives. Subsequently, derivatization of ethynyl-substituted triptycenes was studied to yield the respective propiolic acid and ethynylphosphine derivatives. Characterization of the newly functionalized triptycene derivatives and their regioisomers were carried out using FTIR and multinuclear NMR spectroscopy, mass spectrometry, and elemental analyses techniques. The study of the interaction of these trisubstituted triptycenes with various forms of DNA revealed interesting dependency on the functional groups of the triptycene core to initiate damage or conformational changes in DNA.

Synthesis and Characterization of Chromium Tricarbonyl Complexes of 1-Phenylgermatrane and 1-Phenylazagermatrane. Crystal Structure of [N(CH2CH2O)3GeC6H5]Cr(CO)3

2002 ◽  
Vol 57 (9) ◽  
pp. 993-998 ◽  
Author(s):  
Sergey S. Karlov ◽  
Denis A. Sorokin ◽  
Yuri F. Oprunenko ◽  
Jörg Lorberth ◽  
Galina S. Zaitseva
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Synthesis And Characterization ◽  
Chromium Tricarbonyl ◽  
Elemental Analyses ◽  
Chromium Tricarbonyl Complexes ◽  
C Nmr

The reaction of 1-phenylgermatrane (1) and 1-phenylazagermatrane (2) with Cr(CO)6 affords chromium tricarbonyl complexes [N(CH2CH2O)3GeC6H5]Cr(CO)3 (6) and [N(CH2- CH2NH)3GeC6H5]Cr(CO)3 (7). In contrast, the same reaction of Cr(CO)6 with 1-(9-anthracenyl) germatrane (3) does not proceed. Composition and structures of the 6 and 7 were established by elemental analyses, 1H and 13C NMR spectroscopy and mass spectrometry. The crystal structure of 6 is reported

Synthesis and characterization of N-glucosylated dithiadiazepine derivatives through carbon-sulfur bond formation

2015 ◽  
Vol 21 (5) ◽  
pp. 269-272 ◽  
Author(s):  
Snehal A. Chavan ◽  
Avinash G. Ulhe ◽  
Baliram N. Berad
Keyword(s):  
Bond Formation ◽  
Synthesis And Characterization ◽  
Mass Spectral ◽  
H Nmr ◽  
Chemical Structures ◽  
Elemental Analyses ◽  
New Compounds ◽  
Sulfur Bond ◽  
C Nmr

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.

9-Silyl(-Germyl,-Stannyl) Substituted Derivatives of 1-(9-Fluorenyl)- germatranes. Synthesis, Characterisation, and Crystal Structures

1998 ◽  
Vol 53 (11) ◽  
pp. 1247-1254 ◽  
Author(s):  
Galina S. Zaitseva ◽  
Sergey S. Karlov ◽  
Bettina A. Siggelkow ◽  
Evgeni V. Avtomonov ◽  
Andrei V. Churakov ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Crystal Structures ◽  
Elemental Analyses ◽  
Derivatives Of ◽  
C Nmr

9-Trimethylsilyl- and 9-trimethylgermyl substituted derivatives of 1-(9-fluorenyl)germatranes C13H8(R)Ge(OCH2CH2)3N (1 - 3) (1: R = H; 2: R = Me3Si; 3: R = Me3Ge) were prepared by the reaction of 9-tribromogermyl derivatives of fluorene C13H8(R)GeBr3 (4 - 6) with N(CH2CH2OSnAlk3)3 (7: Alk = Et; 8: Alk = Bu). 1-(9-Trimethylstannyl- 9-fluorenyl)germatrane (14) was synthesised by the reaction o f the germatrane (1) with Me3SnNMe2 . Formulas and structures were established by elemental analyses, (1H, 13C) NMR spectroscopy and mass spectrometry; crystal structures of 2 and 14 are reported.

scholarly journals Synthesis And Single Crystal X-Ray Structure Of 2-(1,3,4-Oxadiazol- 2-yl)Aniline

2007 ◽  
Vol 62 (6) ◽  
pp. 835-840 ◽  
Author(s):  
Ali Souldozi ◽  
Katarzyna Ślepokura ◽  
Tadeusz Lis ◽  
Ali Ramazani
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Structural Analysis ◽  
Single Crystal ◽  
Structure Determination ◽  
High Yield ◽  
Aminobenzoic Acid ◽  
Aromatic Rings ◽  
X Ray ◽  
C Nmr

Reaction of 2-aminobenzoic acid with (N-isocyanimino)triphenylphosphorane proceeds smoothly at r. t. to afford 2-(1,3,4-oxadiazol-2-yl)aniline in high yield. The structure of this compound was confirmed by IR, 1H, and 13C NMR spectroscopy, mass spectrometry, and single crystal X-ray structure determination. The X-ray structural analysis of the product indicated that its aromatic rings are approximately co-planar

Chemistry of the 1,3,5-Triaza-2-phosphorin-4,6-diones, Part XII*. Synthesis and Characterization of 2-PhenyI-2-(p-tolylthio)-1,3,5- trimethyI-1,3,5-triaza-4,6-dione-2-phosphorinonium Salts

1996 ◽  
Vol 51 (10) ◽  
pp. 1494-1500 ◽  
Author(s):  
Vasily A . Pinchuk ◽  
Ion Neda ◽  
Christian Müller ◽  
Holger Thönnessen ◽  
Peter G. Jones ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
New Products ◽  
Synthesis And Characterization ◽  
Tetrahedral Geometry ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Weak Hydrogen Bonds ◽  
C Nmr

The reaction of 1,5-bis(trimethylsilyl)-1,3.5-trimethylbiuret (1) with p-tolylsulfenyl chloride (2) furnished l-(p-tolylthio)-5-trimethylsilyl-1,3,5-trimethylbiuret (3). In the reaction of 3 with phenyldichlorophosphine, 2-phenyl-2-(p-tolylthio)-1,3,5-trimethyl-1,3,5-triaza-4,6-dione- 2-phosphorinonium chloride (4) was formed. The same product was obtained from the reaction of 2-phenyl-1,3,5-trimethyl-1,3,5-triaza-2λ3- phosphorin-4,6-dione (6) with p-tolylsulfenyl chloride (2). Compound 4 was isolated and characterized in the form of the hexachloroantimonate (4a). The spirophosphorane 2-phenyl-1,3,5-trimethyl-1,3,5-triaza-7,10-dioxa-8,9- perchlorobenzo-2λ5-phosphaspiro-[4.5]decan-4,6-dione (7) was prepared by the reaction of 4 with tetrachloroorthobenzoquinone. The new products were characterized by 1H - and 13C NMR spectroscopy, elemental analysis, 31P NMR spectroscopy in the case of 4a. 6 and 7, and mass spectrometry (4a). Single-crystal X-ray structural analyses of compounds 4a and 7 were conducted. The phosphorus atom of 4a has the expected tetrahedral geometry, with a rather short P-S bond of 204.9(2) pm. In 7 the geometry at phosphorus is almost ideal trigonal bipyramidal. Weak hydrogen bonds are formed from a C (:O) group to deuterochloroform of solvation.

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