Carbamoyl and Thiocarbamoyl Derivatives of 3-Aminopropyl-dimethyl-phosphine Oxide

2004 ◽  
Vol 59 (2) ◽  
pp. 221-227 ◽  
Author(s):  
Victoria Lachkova ◽  
Helmut Keck ◽  
Rosario Scopelliti ◽  
Wolfgang Kläui ◽  
Sabi Varbanov ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Phosphine Oxide ◽  
Elemental Analysis ◽  
Phosphine Oxides ◽  
X Ray Diffraction ◽  
X Ray ◽  
H Nmr ◽  
Derivatives Of

A series of fourteen new 3-[N-substituted carbamoyl (or thiocarbamoyl)]-aminopropyl-dimethyl-phosphine oxides have been synthesized and characterized. The compounds were prepared via reaction of the 3-aminopropyl-dimethyl-phosphine oxide with the corresponding isocyanates or isothiocyanates. The composition of the compounds was proved by elemental analysis and the structures were confirmed by IR, 1H, 31P, 31P{1H} NMR spectroscopy and by mass spectrometry. The structures of 3[(N-phenyl-thiocarbamoyl)amino]propyl-dimethyl-phosphine oxide (5), 3[(N-4- chlorophenyl-thiocarbamoyl)amino]propyl-dimethyl-phosphine oxide (6), and 3[(N-benzyl-thiocarbamoyl) amino]propyl-dimethyl-phosphine oxide (9) have been confirmed by X-ray diffraction.

Synthesis of Dimethylphosphinoyl Substituted α-Aminoarylmethanephosphonates

2005 ◽  
Vol 60 (2) ◽  
pp. 215-220 ◽  
Author(s):  
Tsvetanka Cholakova ◽  
Yulian Zagraniarsky ◽  
Gerhard Hägele ◽  
Tania Tosheva ◽  
Bojidarka Ivanova ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Schiff Bases ◽  
Elemental Analysis ◽  
X Ray Diffraction ◽  
X Ray ◽  
H Nmr

New dimethylphosphinoyl-substituted α-aminoarylmethanephosphonates 1a - f have been synthesized via addition of dimethyl or diethyl phosphites to Schiff bases and via Kabachnik-Fields reaction. The structure of the compounds was confirmed by elemental analysis, IR, 1H and 31P{1H} NMR spectroscopy, mass spectrometry and in two cases by X-ray diffraction.

N-Dimethylphosphinoyl-substituted Aminomethanephosphonic Acids

2010 ◽  
Vol 65 (5) ◽  
pp. 556-564 ◽  
Author(s):  
Victoria Lachkova ◽  
Sabi Varbanov ◽  
Walter Frank ◽  
Helmut Keck
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Single Crystal ◽  
Electrospray Ionization ◽  
Elemental Analysis ◽  
Electrospray Ionization Mass Spectrometry ◽  
Ionization Mass ◽  
X Ray Diffraction ◽  
X Ray ◽  
H Nmr

Three new N-phosphinoyl-substituted aminomethanephosphonic acids have been synthesized and characterized: dimethylphosphinoylmethyl-imino-bis(methanephosphonic acid) (1), [3-(dimethylphosphinoyl)-propyl]-imino-bis(methanephosphonic acid) (2), and N-benzyl-Ndimethylphosphinoylmethyl- aminomethanephosphonic acid (3). The latter was isolated as a hydrochloride 3 ・ HCl. The acids have been prepared via Moedritzer-Irani reaction from the corresponding dimethylphosphinoyl-substituted primary and secondary aliphatic amines. Their structures have been confirmed by elemental analysis, IR, 1H, 31P{1H}, 13C{1H} NMR spectroscopy, electrospray ionization mass spectrometry, and single-crystal X-ray diffraction.

scholarly journals Synthesis, Structure, and Properties of a Dinuclear Cu(II) Coordination Polymer Based on Quinoxaline and 3,3-Thiodipropionic Acid Ligands

2021 ◽  
Author(s):  
Adedibu Clement Tella ◽  
Samson Owalude ◽  
Vincent Adimula ◽  
Adetola Oladipo ◽  
Victoria Olayemi ◽  
...  
Keyword(s):  
Nmr Spectroscopy ◽  
Nitrogen Atom ◽  
Coordination Polymer ◽  
Elemental Analysis ◽  
Catalytic Reduction ◽  
Copper Acetate ◽  
Structure And Properties ◽  
X Ray Diffraction ◽  
X Ray ◽  
H Nmr

Abstract The coordination polymer [Cu2(TDPH)4(QNX)].DMF, (QNX = Quinoxaline; TDPH = 3,3-thiodipropionic acid), has been prepared by reaction of copper acetate, TDPH, and quinoxaline. The compound was characterized by elemental analysis, FTIR spectroscopy, and single-crystal X-ray diffraction. The crystal is monoclinic with a P21/n space group and dimensions of a = 12.889(3) Å, b = 14.983(4) Å, c = 14.091(3) Å, α = 90 °, β = 90.200(11) °, γ = 90 °, V = 2721.18 (2) Å3, Z = 4. The ligands are hexagonally coordinated to the Cu(II) centre in the form of Cu2O4N with one nitrogen atom from the quinoxaline ligand, and four oxygen atoms from four TDPH molecules in a monodentate fashion. The Cu-Cu bond length was 2.642(1) and 2.629(1) Å for the Cu1----Cu1 and Cu2----Cu2 bonds. The QNX ligand bridged the two copper atoms. The catalytic reduction of 4-nitrophenol to 4-aminophenol using NaBH4 in the presence of [Cu2(TDPH)4(QNX)].DMF, as catalyst was completed within 11 minutes. The 4-aminophenol product was confirmed using 1H NMR spectroscopy.

Synthesis and crystal structures of two new lead(II) complexes with the pincer-type ligand 4′-(4-chlorophenyl)-2,2′:6′,2″-terpyridine (Cl-Ph-tpy): subtle interplay of weak intermolecular interactions

2020 ◽  
Vol 75 (12) ◽  
pp. 1043-1048
Author(s):  
Farzin Marandi ◽  
Harald Krautscheid
Keyword(s):  
Nmr Spectroscopy ◽  
Single Crystal ◽  
Elemental Analysis ◽  
Central Unit ◽  
X Ray Diffraction ◽  
X Ray ◽  
H Nmr ◽  
Weak Intermolecular Interactions ◽  
Binuclear Structure ◽  
Ft Ir

AbstractA dinuclear and a tetranuclear complex of lead(II) with the pincer-type ligand 4′-(4-chlorophenyl)-2,2′:6′,2″-terpyridine (Cl-Ph-tpy), [Pb2(Cl-Ph-tpy)2(μ-I)2I2] (1) and [Pb4(Cl-Ph-tpy)4(μ-Br)4(μ-OH2)Br4]·2CH3OH (2), have been synthesized and characterized by elemental analysis, FT-IR and 1H NMR spectroscopy, and by single-crystal X-ray diffraction. In the binuclear structure of 1, the Pb atom has a hemidirected PbN3I3 environment with a Pb(μ-I)2Pb central unit. In the tetranuclear structure of 2, two crystallographically independent Pb(II) centres having hemidirected PbN3Br3 and PbN3OBr2 environments are connected to Pb(μ-Br)Pb(μ-Br)2(μ-OH2)Pb(μ-Br)Pb chains. The supramolecular features in 1 and 2 are supported through weak but directional C–H···Cl, C–H···I and C–H···Br, C–H···O, O–H···Br, and O···Br interactions and aromatic π-π stacking.

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.

Synthese und Charakterisierung von Halogen-phosphor(III)- Derivaten des 8-Hydroxychinolins. Röntgenstrukturanalyse von 8-[Phenyl(chloro)-phosphito]-chinolin/ Synthesis and Characterization of Halogen-phosphorus(III) Derivatives of 8-Hydroxyquinoline. X -Ray Structure Analysis of 8-[Phenyl(chloro)phosphito]-quinoline

1993 ◽  
Vol 48 (1) ◽  
pp. 85-89 ◽  
Author(s):  
Lin Yang ◽  
Peter G. Jones ◽  
Reinhard Schmutzler
Keyword(s):  
Nmr Spectroscopy ◽  
Single Crystal ◽  
Diffraction Study ◽  
Elemental Analysis ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
New Compounds ◽  
Derivatives Of

The reaction of 8 -trimethylsiloxyquinoline, 2 with PCl3, PhPCl2, and PhPF2 has furnished the corresponding 8 -quinolyl halophosphite derivatives, 3-5 . The synthesis of two metal complexes, 8 and 9, of 4 with Au(I) and Pt(II) is described. The new compounds were characterized by elemental analysis and by 1H and 31P NMR spectroscopy. A single crystal X-ray diffraction study of 4 has been conducted; a short intramolecular P ··· N contact (230.9 pm) and a long P-Cl bond (218.7 pm) were observed.

scholarly journals Tautomerisation in 1-(4-Methylphenylazo)naphthalen-2-ol and 2-(4-Methylphenylazo)-4-methylphenol: A Crystallographic and 13C{1H}NMR Study

1999 ◽  
Vol 23 (3) ◽  
pp. 178-179
Author(s):  
Wendy I. Cross ◽  
Kevin R. Flower ◽  
Robin G. Pritchard
Keyword(s):  
Acetic Acid ◽  
Nmr Spectroscopy ◽  
Resonant Frequency ◽  
X Ray Diffraction ◽  
X Ray ◽  
H Nmr ◽  
Nmr Study ◽  
Acetic Acid Esters ◽  
Acid Esters ◽  
Equivalent Carbon

The acetic acid esters of 1-(4-methylphenylazo)naphthalen-2-ol 1 and 2-(4-methylphenylazo)-4-methylphenol 3 are prepared and characterised by single crystal X-ray diffraction studies and 13C{1H}NMR spectroscopy; the position of the C(2)13C resonance for the ester is used to predict the position of resonant frequency of the equivalent carbon in the parent alcohols and hence, calculate the position of the azo-hydrazone equilibrium in these compounds.

scholarly journals Exploring the Structural Chemistry of Pyrophosphoramides: N,N′,N″,N‴-Tetraisopropylpyrophosphoramide

Chemistry ◽  
2021 ◽  
Vol 3 (1) ◽  
pp. 149-163
Author(s):  
Duncan Micallef ◽  
Liana Vella-Zarb ◽  
Ulrich Baisch
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
Nuclear Magnetic Resonance ◽  
Hydrogen Bonding ◽  
Nmr Spectroscopy ◽  
Ir Spectroscopy ◽  
Room Temperature ◽  
Intermolecular Hydrogen Bonding ◽  
X Ray Diffraction ◽  
X Ray

N,N′,N″,N‴-Tetraisopropylpyrophosphoramide 1 is a pyrophosphoramide with documented butyrylcholinesterase inhibition, a property shared with the more widely studied octamethylphosphoramide (Schradan). Unlike Schradan, 1 is a solid at room temperature making it one of a few known pyrophosphoramide solids. The crystal structure of 1 was determined by single-crystal X-ray diffraction and compared with that of other previously described solid pyrophosphoramides. The pyrophosphoramide discussed in this study was synthesised by reacting iso-propyl amine with pyrophosphoryl tetrachloride under anhydrous conditions. A unique supramolecular motif was observed when compared with previously published pyrophosphoramide structures having two different intermolecular hydrogen bonding synthons. Furthermore, the potential of a wider variety of supramolecular structures in which similar pyrophosphoramides can crystallise was recognised. Proton (1H) and Phosphorus 31 (31P) Nuclear Magnetic Resonance (NMR) spectroscopy, infrared (IR) spectroscopy, mass spectrometry (MS) were carried out to complete the analysis of the compound.

An Intramolecular Boron Nitrogen Lewis Acid Base Pair on a Rigid Naphthyl Backbone

2012 ◽  
Vol 67 (6) ◽  
pp. 589-593 ◽  
Author(s):  
Daniel Winkelhaus ◽  
Beate Neumann ◽  
Norbert W. Mitzel
Keyword(s):  
Nmr Spectroscopy ◽  
Single Crystal ◽  
Lewis Acid ◽  
Elemental Analysis ◽  
Base Pair ◽  
Ring System ◽  
X Ray Diffraction ◽  
Acid Base ◽  
X Ray ◽  
Boron Nitrogen

The reaction of (C6F5)2BCl with 8-lithio-N,N-dimethyl-1-naphthylamine (1) afforded the fivemembered ring system 8-bis(pentafluorophenyl)boryl-N,N-dimethyl-1-naphthylamine (2) with an intramolecular dative B-N bond. The compound was characterised by elemental analysis, NMR spectroscopy and single-crystal X-ray diffraction.

[Zn(phen)2(CX3COO)]+, X = H orCl; Influence of X on the Coordination Mode of the Carboxylate Group (phen = 1,10-Phenanthroline)

2005 ◽  
Vol 60 (10) ◽  
pp. 1049-1053 ◽  
Author(s):  
Zeanab Talaei ◽  
Ali Morsali ◽  
Ali R. Mahjoub
Keyword(s):  
Nmr Spectroscopy ◽  
Elemental Analysis ◽  
Coordination Mode ◽  
Bidentate Ligand ◽  
Carboxylate Group ◽  
X Ray ◽  
X Ray Crystallography ◽  
H Nmr ◽  
Coordinate Geometry ◽  
C Nmr

Two new ZnII(phen)2 complexes with trichloroacetate and acetate anions, [Zn(phen)2(CCl3COO)- (H2O)](ClO4) and [Zn(phen)2(CH3COO)](ClO4), have been synthesized and characterized by elemental analysis, IR, 1H NMR, 13C NMR spectroscopy. The single crystal X-ray data of these compounds show the Zn atoms to have six-coordinate geometry. From IR spectra and X-ray crystallography it is established that the coordination of the COO− group is different for trichloroacetate and acetate. The former acts as a monodentate whereas the latter acts as a bidentate ligand.

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