Synthesis and Crystal Structure of Schiff Bases Based on AMTTO (AMTTO = 4-Amino-6-methyl-3-thio-3,4-dihydro-1,2,4-triazin- 5(2H)-one)

2006 ◽  
Vol 61 (11) ◽  
pp. 1421-1425 ◽  
Author(s):  
Maasoomeh Tabatabaee ◽  
Mitra Ghassemzadeh ◽  
Behnaz Zarabi ◽  
Bernhard Neumüllerc
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Microwave Irradiation ◽  
Schiff Bases ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Ir And Nmr Spectroscopy

Reaction of 4-amino-6-methyl-3-thio-3,4-dihydro-1,2,4-triazin-5(2H)-one (1) with 2-methoxybenzaldehyde, 4-methoxybenzaldehyde, 2-pyridinecarbaldehyde, and 2,4-dichlorobenzaldehyde under classical heating and microwave irradiation in a solventfree system led to the corresponding imines (Schiff bases) 2-5. All synthesized compounds have been characterized by IR and NMR spectroscopy, mass spectrometry and by X-ray diffraction studies.

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.

scholarly journals Synthesis and Crystal Structure of Unexpected (1S,4R,5R,6S)-4-Cyano-2,2,6-trimethyl-3-azabicyclo[3.3.1]nonan-6-yl Acetate

2017 ◽  
Vol 70 (12) ◽  
pp. 1269
Author(s):  
Steven Gareth Williams ◽  
Mohan Bhadbhade ◽  
Roger Bishop ◽  
Alison Thavary Ung
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
High Resolution Mass Spectrometry ◽  
Unit Cell Parameters ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Cell Parameters ◽  
X Ray Crystallography ◽  
Ir And Nmr Spectroscopy ◽  
Resolution Mass

The reaction of (–)-β-pinene with KCN under a mild bridged Ritter reaction gave (1S,5R,6S)-2,2,6-trimethyl-3-aza-bicyclo[3.3.1]non-3-en-6-yl acetate that subsequently reacted to provide an unexpected (1S,4R,5R,6S)-4-cyano-2,2,6-trimethyl-3-azabicyclo[3.3.1]nonane-6-yl acetate. The structure of the compound was determined by high-resolution mass spectrometry, and IR and NMR spectroscopy and confirmed by single crystal X-ray crystallography. The compound crystallises in the monoclinic P21 space group, with unit cell parameters a 8.6120 (17), b 7.4570 (15), c 11.189 (2) Å, and β 110.16 (3)°.

Synthesis and Crystal Structure of (1E,2E)-1,2-Di (-3-Nitrobenzylidene) Hydrazine under Micromave Irradiation

2013 ◽  
Vol 787 ◽  
pp. 205-207
Author(s):  
Hong Yan Zhou
Keyword(s):  
Crystal Structure ◽  
Microwave Irradiation ◽  
Monoclinic Space Group ◽  
Stacking Interactions ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
H Nmr ◽  
The Stability ◽  
High Yields

A compound of (1E,2E)-1,2-di (-3-nitrobenzylidene) hydrazine was synthesized under microwave irradiation (500 w), giving high yields of products (93%). Its structure was determined IR, 1H NMR, MS, elemental analysis and X-ray diffraction. The crystal of the compound is Monoclinic, space group P2(1)/n with a = 6.9611(18), b = 7.823(2), c = 12.999(3) Å, α = 90, β = 105.215(4), γ = 90o, V= 683.1(3) Å3, Z=4, Dc=1.450g/cm3,μ=0.110 mm-1, F(000)=308, R=0.0401 and wR = 0.1131 for 1273 observed reflection with I>2σ (I). π-π stacking interactions contribute to the stability of the structure.

scholarly journals Palladium(II) complexes with R2edda derived ligands, Part III: Diisobutyl (s,s)-2,2'-(1,2-ethanediyldiimino)di(4-methylpentanoate) and its palladium(II) complex: Synthesis and characterization

2009 ◽  
Vol 74 (11) ◽  
pp. 1249-1258 ◽  
Author(s):  
Bojana Zmejkovski ◽  
Goran Kaludjerovic ◽  
Santiago Gómez-Ruiz ◽  
Tibor Sabo
Keyword(s):  
Crystal Structure ◽  
Nmr Spectroscopy ◽  
Hydrogen Bonds ◽  
Nmr Spectra ◽  
Symmetry Axis ◽  
Layer Structure ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
Ir And Nmr Spectroscopy

A new R2edda-type ester, diisobutyl (S,S)-2,2'-(1,2-ethane-diyldiimino) di(4-methylpentanoate) dihydrochloride, [(S,S)-H2iBu2eddl]Cl2, 1, and its palladium(II) complex, dichloro(diisobutyl (S,S)-2,2'-(1,2-ethanediyldiimino) di(4-methylpentanoate))palladium(II), [PdCl2{(S,S)-iBu2eddl}], 2, were synthesized and characterized by elemental analysis, as well as IR and NMR spectroscopy. It was found that complex 2 was obtained as mixture of two diastereoisomers, observed in NMR spectra. The crystal structure of compound 1 was determined by X-ray diffraction studies and is described. The isolated crystals consisted of one dicationic species [(S,S)-H2iBu2eddl]2+ and two Cl-. The crystal system was tetragonal with the space group P42. Hydrogen bonds significant for the manner of packing are N-H1N???Cl, 3.049(3) ?, 159(3)? and N-H2N???Cl, 3.100(3) ?, 164(3)?. An infinite chain was formed building a one layer structure, usual for these types of compounds. The C2 symmetry axis of the compound passes through the C1-C1i bond vector and lies perpendicular to the plane N2Cl2.

Dimeres Di(N-lithium–tert–butylamino)bis(dimethylamino)silan - [Si(N(CH3)2)2(NLiC(CH3)3)2]2 – Darstellung und Kristallstruktur / Dimeric Di(N -lithio-tert-butylamino)bis(dimethylamino)silane - [Si(N(CH3)2)2(NLiC(CH3)3)2]2 – Synthesis und Crystal Structure

2001 ◽  
Vol 56 (1) ◽  
pp. 90-94 ◽  
Author(s):  
Josef Engering ◽  
Eva-Maria Peters ◽  
Martin Jansen
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
Solid State ◽  
Nmr Spectroscopy ◽  
Single Crystal ◽  
Title Compound ◽  
Solution Nmr ◽  
X Ray Diffraction ◽  
X Ray ◽  
Solution Nmr Spectroscopy

Abstract [Si(N(CH3)2)2(NLiC(CH3)3)2]2 results from the reaction of silicon tetrachloride with excess terf-butylamine, followed by halogen substitution with LiN(CH3)2, and treatment with n-butyllithium in hexane. The title compound, found to be dimeric in the solid state, was characterised by single crystal X-ray diffraction (triclinic, Pi , a = 10.208(2), b = 12.140(2), c = 15.658(3) Å , a = 79.02(3), ß = 82.80(3), γ = 67.19(3)°, Z = 2, C24H60Li4N8Si2 ), and by solid state and solution NMR-spectroscopy and mass spectrometry.

The first example of the stereoselective synthesis and crystal structure of a spirobicycloquinazolinone based on (–)-fenchone and anthranilamide

2019 ◽  
Vol 75 (12) ◽  
pp. 1675-1680 ◽  
Author(s):  
Vladimir V. Chernyshov ◽  
Yuri V. Gatilov ◽  
Olga I. Yarovaya ◽  
Igor P. Koskin ◽  
Spartak S. Yarovoy ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Nmr Spectroscopy ◽  
Unit Cell Volume ◽  
Stereoselective Synthesis ◽  
Stacking Interactions ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
First Time ◽  
C Nmr

The possibility of a single-stage solvent-free stereoselective synthesis of a spirocyclic compound from the natural bicyclic monoterpenoid (−)-fenchone and anthranilamide has been shown for the first time. The molecular and crystal structure of (1R,2S,4S)-1,3,3-trimethyl-1′H-spiro[bicyclo[2.2.1]heptane-2,2′-quinazolin]-4′(3′H)-one, C17H22N2O, was established by X-ray diffraction though the chirality was assumed via the known reactant connectivity and 1H and 13C NMR spectroscopy. It has shown that in the molecule, for steric reasons, there is an elongation of the Me2C—C(N)N bond to 1.603 (5) Å. The formation of dimers via N—H...O=C hydrogen bonds with an interaction energy of 93.30 kJ mol−1 and through cavities (33.7% of the unit-cell volume) was established in the packing of the molecules. There are no π-stacking interactions in the structure.

Synthesis and crystal structure of a homoleptic diruthenium complex containing tetra-2-pyridyl-1,4-pyrazine (tppz)

2017 ◽  
Vol 72 (10) ◽  
pp. 759-762 ◽  
Author(s):  
Marion Graf ◽  
Peter Mayer ◽  
Hans-Christian Böttcher
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Title Complex ◽  
Dinuclear Complex ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
X Ray Crystallography ◽  
Diruthenium Complex

AbstractTreatment of hydrated ruthenium(III) chloride with tetra-2-pyridyl-1,4-pyrazine (tppz) in refluxing ethoxyethanol afforded the homoleptic dinuclear complex [(tppz)Ru(μ-tppz)Ru(tppz)]4+ (1) besides small amounts of the species [Ru(tppz)2]2+. The title complex 1 was obtained as purple crystals and characterized as its hexafluoridophosphate salt by NMR spectroscopy, mass spectrometry and microanalyses. The molecular structure of 1(PF6)4 has been established by X-ray crystallography.

Synthesis, Characterization, Crystal Structure, and Cytotoxicity of a 7-Coordinate Diorganotin(IV) Complex of 2-Acetylpyrazine N4-Methylthiosemicarbazone

2012 ◽  
Vol 67 (2) ◽  
pp. 149-153 ◽  
Author(s):  
Xian Feng Zhu ◽  
Li Zhi Zhang ◽  
Min Yang ◽  
Yan Ke Li ◽  
Ming Xue Li
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
X Ray Diffraction ◽  
Leukaemia Cell ◽  
Leukaemia Cell Line ◽  
X Ray ◽  
Thiosemicarbazone Ligand ◽  
Biological Studies

The diorganotin(IV) complex [Ph2Sn(L)(CH3COO)] (1), where HL = 2-acetylpyrazine N4-methyl thiosemicarbazone, has been synthesized and characterized by elemental analysis, IR, UV/Vis and NMR spectroscopy, mass spectrometry, and single-crystal X-ray diffraction. Complex 1 contains mononuclear neutral molecules composed of one N2S tridentate anionic thiosemicarbazone ligand, one acetato group, and one Ph2Sn(IV) group with a seven-coordinated tin atom. In vitro biological studies have indicated that complex 1 shows effective cytotoxicity with IC50 = 5.4 μM against the K562 leukaemia cell line.

Notizen: Synthese und Kristallstruktur von [{(CO)5CrPhP}2Se3] / Synthesis and Crystal Structure of [{(CO)5CrPhP}2Se3]

1992 ◽  
Vol 47 (11) ◽  
pp. 1649-1652 ◽  
Author(s):  
Kurt Merzweiler ◽  
Hans-Jörg Kersten
Keyword(s):  
Crystal Structure ◽  
Nmr Spectroscopy ◽  
Single Crystal ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
X Ray

The reaction of [{(CO)5Cr}PhPCl2] with Se(SiMe3)2 leads to the formation of [{(CO)5CrPhP}2Se3] (1). 1 contains a P2Se3-heterocycle which is coordinated to two {(CO)5Cr} units. 1 was characterized by NMR spectroscopy (31P, 77Se) and single crystal 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.

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