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.

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 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.

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.

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 and Characterization of a Series of 1-Aryl-4-[aryldiazenyl]- piperazines. Part I. Isomers of N-(2,3-Dimethylphenyl)-N’-(Aryldiazenyl)- Piperazines

2015 ◽  
Vol 2 (1) ◽  
pp. 20-35
Author(s):  
Chenguang Fan ◽  
Keith Vaughan
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Synthesis And Characterization ◽  
Ir And Nmr Spectroscopy ◽  
Common Thread ◽  
Diazonium Coupling ◽  
New Compounds

This paper describes the synthesis of several new series of 1-(2-aryldiazen-1-yl-) 4-arylpiperazines and 1-(2- aryldiazen-1-yl-)4-arylalkylpiperazines by using diazonium coupling between arenediazonium ions with the appropriate 1-arylpiperazine or the 1-arylalkylpiperazine. The new compounds have a common thread in that they are isomers of the series of N-(2,3-dimethylphenyl)- N’-(aryldiazenyl)-piperazines. The new triazenes have been characterized by IR and NMR spectroscopy and mass spectrometry.

Synthesis and characterization of a porphyrin-crown ether conjugate as a potential intermediate for drug delivery application

2020 ◽  
pp. A-G
Author(s):  
Maher Fathalla
Keyword(s):  
Mass Spectrometry ◽  
Drug Delivery ◽  
High Resolution Mass Spectrometry ◽  
Mesoporous Silica Nanoparticles ◽  
Synthesis And Characterization ◽  
Delivery Vehicle ◽  
Potential Applications ◽  
Resolution Mass ◽  
C Nmr

The development of synthetic strategies for functional building units plays a central role in supramolecular chemistry. Both porphyrin and crown ethers have attracted the attention of researchers worldwide owing to their unique properties. It is envisioned that the integration of the two molecules will result in hybrid materials with potential applications in many fields. In the present study, a new porphyrin derivative 3 appended with four 18-crown-6 (18C6) ether moieties was synthesized through the Suzuki-Miyaura coupling of boronic ester porphyrin 1 and 4-bromobenzo-18-crown-6 2 in 80% yield. Porphyrin 3 was fully characterized by 1H/[Formula: see text]C NMR spectroscopy and high resolution mass spectrometry. The tendency of the 18C6 to form host-guest complexes with ammonium cations was exploited to assemble cation responsive hybrid material of porphyrin 3 and ammonium immobilized mesoporous silica nanoparticles (MSNs). Furthermore, the potential application of the 3/MSNs conjugate as a cation-responsive drug delivery vehicle was investigated in solution by UV-vis and fluorescence spectroscopies.

Synthesis and characterization of various unsubstituted and mono-N-substituted tetraazamacrocycles

1995 ◽  
Vol 73 (5) ◽  
pp. 685-695 ◽  
Author(s):  
I. Meunier ◽  
A.K. Mishra ◽  
B. Hanquet ◽  
R. Guilard ◽  
P. Cocolios
Keyword(s):  
Mass Spectrometry ◽  
Template Synthesis ◽  
2D Nmr ◽  
Spectral Studies ◽  
Synthesis And Characterization ◽  
Difference Spectroscopy ◽  
Protective Group ◽  
Noe Difference Spectroscopy ◽  
C Nmr

Syntheses of tetraazamacrocycles have been carried out by using p-toluenesulfonyl chloride as protective group. The [14(ane) N4] and [15(ane) N4] were also obtained by the template synthesis. Mono-N-functionalization of tetraazamacrocycles was accomplished by reaction of a fivefold excess of the free macrocycles with 1 equivalent of a suitable alkylating or arylating reagent. The key point of the synthesis lies in the use of an excess of the macrocycle over the substituting reactants to reduce the formation of polysubstituted derivatives, and in the easy separation of the excess of unreacted macrocycle. All the products were characterized on the basis of spectral studies (1H and l3C NMR, including 2D NMR and NOE difference studies) and mass spectrometry. Keywords: tetraazamacrocycles, improved synthesis, protective group, N-tosylation, template synthesis, NOE difference spectroscopy.

The Synthesis and Characterization of Nitrooxy- and Nitrosooxyborazine Compounds

2014 ◽  
Vol 69 (11-12) ◽  
pp. 1241-1247
Author(s):  
Thomas M. Klapötke ◽  
Magdalena Rusan
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Vibrational Spectroscopy ◽  
Elemental Analysis ◽  
Experimental Results ◽  
Synthesis And Characterization ◽  
The Impact

Abstract B-Nitrosooxypentamethylborazine, B-nitrooxypentamethylborazine and B-trinitrooxy-N-trimethylborazine have been synthesized and characterized by 1H, 13C, 11B, and 14N NMR spectroscopy, mass spectrometry, vibrational spectroscopy and elemental analysis. The 11B NMR shifts were calculated and compared to the experimental results. The decomposition temperatures and the impact and friction sensitivities of these compounds have been determined as well.

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