scholarly journals Mass Spectrometry Reveals Complexing Properties of Modified PNP-Lariat Ether Containing Benzyl Derivative of (S)–Prolinamine

Molecules ◽  
2019 ◽  
Vol 25 (1) ◽  
pp. 136 ◽  
Author(s):  
Natalia Gutowska ◽  
Piotr Seliger ◽  
Jarosław Romański ◽  
Magdalena Zięba ◽  
Grazyna Adamus ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Crown Ether ◽  
Coordination Polymers ◽  
Elemental Analysis ◽  
Structural Unit ◽  
Optically Active ◽  
Lariat Ether ◽  
Complexing Properties ◽  
Complexation Ability

In the investigation presented here the synthesis of new lariat ether derivative obtained from the modification of tetrapyrrolidinyl-PNP-crown ether macrocycle is described. The polyheterotopic molecular coreceptor consisted of the replacement of chlorine atoms with an optically active (S)-(1-benzylpyrrolidin-2-yl) methanamine. The structure was confirmed by using elemental analysis, mass spectrometry, and NMR spectroscopy. This work covers results concerning the complexing properties of the new ligand towards Ag+, Cu2+, Co2+, Ni2+, and Zn2+ ions. The formation of non-covalent complexes of 1:1 stoichiometry with the Cu2+, Co2+, Ni2+, and Zn2+ ions have been confirmed by mass spectrometry. Due to the previous work and application possibilities, a large emphasis was put on the investigation of the complexation ability of lariat ether with silver (I) cation to determine stability constants by direct potentiometric method. In this case, the formation of four different forms of complexes AgL, Ag2L, Ag3L, and Ag4L has been proved. The observed unusual binding through the nitrogen atoms from the exocyclic substituents may provide the structural unit to build a new coordination polymers.

scholarly journals Ambient-Temperature Synthesis of (E)-N-(3-(tert-Butyl)-1-methyl-1H-pyrazol-5-yl)-1-(pyridin-2-yl)methanimine

Molbank ◽  
10.3390/m1250 ◽  
2021 ◽  
Vol 2021 (3) ◽  
pp. M1250
Author(s):  
Diana Becerra ◽  
Justo Cobo ◽  
Juan-Carlos Castillo
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Ambient Temperature ◽  
Magnesium Sulfate ◽  
Elemental Analysis ◽  
Condensation Reaction ◽  
2D Nmr ◽  
2D Nmr Spectroscopy ◽  
Temperature Synthesis ◽  
Tert Butyl

We report the ambient-temperature synthesis of novel (E)-N-(3-(tert-butyl)-1-methyl-1H-pyrazol-5-yl)-1-(pyridin-2-yl)methanamine 3 in 81% yield by a condensation reaction between 3-(tert-butyl)-1-methyl-1H-pyrazol-5-amine 1 and 2-pyridinecarboxaldehyde 2 in methanol using magnesium sulfate as a drying agent. The N-pyrazolyl imine 3 was full characterized by IR, 1D, and 2D NMR spectroscopy, mass spectrometry, and elemental analysis.

Polynuclear Gold(I) Complexes of Dendritic Amines: Formation of Terminal Tris[(triphenylphosphine)aurio(I)]ammonium Groups -N(AuPPh3)31+

1994 ◽  
Vol 49 (6) ◽  
pp. 781-787 ◽  
Author(s):  
Peter Lange ◽  
Holger Beruda ◽  
Wolfgang Hiller ◽  
Hubert Schmidbaur
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Elemental Analysis ◽  
Spectroscopic Data ◽  
Chemical Properties ◽  
Crystalline Solids ◽  
High Yields

The reactions of dendritic amines RN(CH2CH2CH2NH2)2 (R = Me, c-Hex, PhCH2) and N(CH2CH2NH2)3 with tris[(triphenylphosphine)aurio(I)]oxonium tetrafluoroborate [O(AuPPh3)3]+BF4- in THF yield species with terminal imido cluster groups -N(AuPPh3)31+. The compounds have been obtained as stable crystalline solids in high yields and characterized by NMR spectroscopy as well as mass spectrometry and elemental analysis. The triply charged nonanuclear complex [N(CH2CH2N(AuPPh3)3)3]3+ exhibits major changes in the 1H spectroscopic data and in the chemical properties as compared with com pounds with dications [RN(CH2CH2CH2N(AuPPh3)3)2]2+ (R = Me, c-Hex, PhCH2). Excessive auration to give hypercoordinated species has not been observed

Rhodium(I)–(N-heterocyclic carbene)–diphosphine complexes

2009 ◽  
Vol 87 (9) ◽  
pp. 1248-1254 ◽  
Author(s):  
Hongsui Sun ◽  
Xiao-Yan Yu ◽  
Paolo Marcazzan ◽  
Brian O. Patrick ◽  
Brian R. James
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Elemental Analysis ◽  
Benzene Solution ◽  
H Nmr ◽  
Diphosphine Dioxide

Reactions of [RhCl(COE)(IPr)]2 (1) and [RhCl(COE)(IMes)]2 (2) (COE = cyclooctene; IPr = N,N′-bis(2,6-diisopropylphenyl)imidazolin-2-ylidene; IMes = N,N′-bis(2,4,6-trimethylphenyl)imidazolin-2-ylidene) with the diphosphines Ph2P(CH2)nPPh2 and 1,2-bis(diphenylphosphino)benzene (dppbz) give the N-heterocyclic carbene (NHC) – diphosphine – rhodium(I) complexes: RhCl(NHC)[Ph2P(CH2)nPPh2] [NHC = IPr, n = 1 (3); NHC = IMes, n = 1 (4); NHC = IPr, n = 2 (5); NHC = IMes, n = 2 (6); NHC = IPr, n = 4 (7); NHC = IMes, n = 4 (8)] and RhCl(NHC)(dppbz) [NHC = IPr (9); NHC = IMes (10)]. All the complexes are characterized by 1H, 31P{1H}, and 13C{1H} NMR spectroscopy, elemental analysis, and mass spectrometry. Complexes 3, 7, and 9 are also characterized crystallographically. In benzene solution, the complexes decompose in the presence of O2 with formation of the diphosphine dioxide, whereas reaction with CO leads to replacement of the NHC ligand to give known carbonyl–diphosphine complexes.

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.

scholarly journals Synthesis and Characterization of New Optically Active Poly (ethyl L-lysinamide)s and Poly (ethyl L-lysinimide)s

2010 ◽  
Vol 2010 ◽  
pp. 1-6 ◽  
Author(s):  
Saeed Zahmatkesh ◽  
Mohammad Reza Vakili
Keyword(s):  
Nmr Spectroscopy ◽  
Elemental Analysis ◽  
Specific Rotation ◽  
Viscosity Measurement ◽  
Optically Active ◽  
Inherent Viscosity ◽  
Synthesis And Characterization

Ethyl L-lysine dihydrochloride was reacted with three different dianhydrides to yield the poly (ethyl L-lysinimide)s ( NMR spectroscopy, elemental analysis, WAX diffraction, TGA, inherent viscosity measurement, and specific rotation.

Synthesis, crystal structure, aggregation-induced emission (AIE) and electroluminescence properties of a novel emitting material based on pyrrolo[3,2-b]pyrrole

2020 ◽  
Vol 8 (40) ◽  
pp. 14208-14218
Author(s):  
Hongbo Wang ◽  
Jinnan Huo ◽  
Hongbo Tong ◽  
Xuehong Wei ◽  
Ying Zhang ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Elemental Analysis ◽  
Donor Group ◽  
Aggregation Induced Emission ◽  
X Ray ◽  
X Ray Crystallography

A novel electroluminescent material based on pyrrolo[3,2-b]pyrrole as skeleton and donor group and dimesitylborons as accept groups has been synthesized and characterized by elemental analysis, mass spectrometry, NMR spectroscopy and X-ray crystallography.

scholarly journals Design, synthesis and spectroscopic properties of crown ether-capped dibenzotetraaza[14]annulenes

2019 ◽  
Vol 15 ◽  
pp. 617-622 ◽  
Author(s):  
Krzysztof Miroslaw Zwoliński ◽  
Julita Eilmes
Keyword(s):  
Nmr Spectroscopy ◽  
Crown Ether ◽  
Elemental Analysis ◽  
Binding Sites ◽  
Spectroscopic Properties ◽  
Design Synthesis ◽  
Face To Face ◽  
C Nmr

The first crown ether-capped dibenzotetraaza[14]annulenes (DBTAAs), featuring two macrocyclic binding sites fixed in a face-to-face orientation, were synthesized in satisfactory 26–28% isolated yields. Direct N-alkylation of 1,4,10-trioxa-7,13-diazacyclopentadecane by symmetric DBTAA derivatives bearing bromoalkoxy pendants proceed smoothly at a reasonable level of dilution (1.25 mM). The structures were fully characterized by HR-ESIMS, FTIR-ATR, 1H and 13C NMR spectroscopy and elemental analysis.

scholarly journals Synthesis and fungicidal activity of novel imidazo[4, 5-b]pyridine derivatives

2019 ◽  
Vol 25 (1) ◽  
pp. 8-14
Author(s):  
Daoxin Wu ◽  
Minhua Liu ◽  
Zhong Li ◽  
Mingming Dang ◽  
Xingping Liu ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Elemental Analysis ◽  
Fungicidal Activity ◽  
Structure Activity Relationship ◽  
Activity Relationship ◽  
Pyridine Derivatives ◽  
Structure Activity ◽  
Puccinia Polysora

AbstractA series of novel imidazo[4,5-b]pyridine derivatives were synthesized and their structures were characterized by NMR spectroscopy, mass spectrometry and elemental analysis. The results of bioassays showed that some compounds exhibit good fungicidal activity against Puccinia polysora In particular, compound 7b showed an EC50 value of 4.00 mg/L, which was comparable with that of tebuconazole. Besides, preliminary structure-activity relationship was discussed.

Gold(I) Complexes of Secondary and Tertiary Amines. Crystal Structure of Triphenylphosphineaurio(I)qinuclidinium Tetrafluoroborate

1992 ◽  
Vol 47 (9) ◽  
pp. 1255-1260 ◽  
Author(s):  
Andreas Grohmann ◽  
Jürgen Riede ◽  
Hubert Schmidbaur
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Secondary Amine ◽  
Tertiary Amine ◽  
Elemental Analysis ◽  
Ammonium Salts ◽  
Tertiary Amines ◽  
Average Value ◽  
Ir And Nmr Spectroscopy

The secondary amine piperidine and the tertiary amine quinuclidine (l-azabicyclo[2.2.2]-octane) were reacted in THF with one equivalent of triphenylphosphinegold(I) tetrafluoroborate, [Ph3PAu]+ BF4-, to give the monoaurated ammonium salts of formula [RnNH(3-n)AuPPh3]+ BF4- (n = 2, 3). The compounds were obtained as crystalline solids in good yields, and were characterized by IR and NMR spectroscopy as well as mass spectrometry and elemental analysis. The crystal structure of the quinuclidinium salt was determined (space group Pbca, Z = 8). The analysis shows independent formula units with no intermolecular Au • • • Au contacts. The Au(I)– N bond (2.11(1) A) is significantly longer than the average value found in poly-aurated ammonium salts.

scholarly journals Metallation of tetradentate N2O2 Schiff base with Mn(II), Co(II), Cu(II) and Zn(II): synthesis, characterization and formation constants measurement

2010 ◽  
Vol 8 (2) ◽  
pp. 291-299 ◽  
Author(s):  
Mozaffar Asadi ◽  
Maryam Mohammadikish ◽  
Khosro Mohammadi
Keyword(s):  
Mass Spectrometry ◽  
Schiff Base ◽  
Ionic Strength ◽  
Nmr Spectroscopy ◽  
Elemental Analysis ◽  
1H Nmr Spectroscopy ◽  
Formation Constants ◽  
Free Energies ◽  
Schiff Base Ligands ◽  
Ft Ir

AbstractFour Schiff base ligands, salabza-H2 = N,N′-bis(salicylidene)-2-aminobenzylamine, were synthesized by condensation of one mole of 2-aminobenzylamine and two moles of salicylaldehyde and/or two moles of substituted salicylaldehyde (5-OMe, 5-Br, 5-NO2). All the four Schiff bases and their Mn(II), Co(II), Cu(II) and Zn(II) complexes are characterized by UV-Vis, FT-IR, 1H NMR spectroscopy, mass spectrometry and elemental analysis. The formation constants and the Gibbs free energies were measured spectrophotometrically for 1:1 complexes in methanol in constant ionic strength (I = 0.1 mol dm−3 NaClO4) and at 25°C. The data refinement was carried out with the SQUAD program. The trend of formation constants of H2L1 with M(II) follows the order: Mn(II) (3.97) Also, the trend of formation constants of ligand toward a given metal (for example Mn) is as follows: H2L1 (p-OMe) (3.97) > H2L2 (p-H) (3.65) > H2L3 (p-Br) (3.37) > H2L4 (p-NO2) (3.04)

Sign in / Sign up

Export Citation Format

Share Document