scholarly journals Green synthesis and structural characterization of novel N1-substituted 3,4-dihydropyrimidin-2(1H)-ones

2019 ◽  
Vol 8 (1) ◽  
pp. 230-234 ◽  
Author(s):  
Min Wang ◽  
Shun Zhang ◽  
Hong X. Jiang ◽  
Hao H. Zhang
Keyword(s):  
Catalytic Activity ◽  
Reaction Mechanism ◽  
Aromatic Aldehydes ◽  
Single Crystal Diffraction ◽  
X Ray ◽  
H Nmr ◽  
Solvent Free Conditions ◽  
Biginelli Condensation ◽  
C Nmr

Abstract Novel N1-substituted 3,4-dihydropyrimidin-2(1H)-one derivatives were synthesized through Biginelli condensation of aromatic aldehydes, β-ketoesters, and monosubstituted (thio)ureas in the presence of copper methanesulfonate at 90°C under solvent-free conditions. The screening of the catalysts showed the copper methanesulfonate was the best. Its catalytic activity remained after three times of use. The products were characterized by IR, 1H NMR, 13C NMR, elemental analysis, and X-ray single crystal diffraction technique. A reasonable reaction mechanism was proposed.

scholarly journals Synthesis and characterization of a new bis-NHC palladium complex and its catalytic activity in the Mizoroki–Heck reaction

2020 ◽  
Vol 44 (11-12) ◽  
pp. 684-688
Author(s):  
Can Feng ◽  
Cheng-xin Liu ◽  
Yu-fang Wang ◽  
Jin Cui ◽  
Ming-jie Zhang
Keyword(s):  
Palladium Complex ◽  
Coupling Reaction ◽  
Aryl Halides ◽  
Heck Coupling ◽  
X Ray ◽  
X Ray Crystallography ◽  
H Nmr ◽  
Excellent Stability ◽  
C Nmr

A new bis- N-heterocyclic carbene palladium complex, (C13H9N2F2)2PdCl2, is synthesized by a three-step reaction and characterized by 1H NMR and 13C NMR spectroscopy as well as by X-ray crystallography. This new bis- N-heterocyclic carbene palladium complex has excellent stability and is capable of efficiently catalyzing the Mizoroki–Heck coupling reaction of aryl halides with acrylates.

Design, preparation and characterization of a new ionic liquid, 1,3-disulfonic acid benzimidazolium chloride, as an efficient and recyclable catalyst for the synthesis of tetrahydropyridine under solvent-free conditions

RSC Advances ◽  
2015 ◽  
Vol 5 (83) ◽  
pp. 67405-67411 ◽  
Author(s):  
Mohsen Abbasi
Keyword(s):  
Ionic Liquid ◽  
Mass Spectra ◽  
Recyclable Catalyst ◽  
Solvent Free ◽  
Disulfonic Acid ◽  
H Nmr ◽  
Solvent Free Conditions ◽  
Ft Ir ◽  
C Nmr

In the present work, 1,3-disulfonic acid benzimidazolium chloride as a new ionic liquid, is synthesized, and characterized by studying its FT-IR, 1H NMR, 13C NMR as well as mass spectra.

Synthesis and characterization of novel azo-embedded N-confused tetraphenylporphyrin

2009 ◽  
Vol 13 (02) ◽  
pp. 215-222 ◽  
Author(s):  
Motoki Toganoh ◽  
Takayoshi Hihara ◽  
Kentaro Yonekura ◽  
Yuichi Ishikawa ◽  
Hiroyuki Furuta
Keyword(s):  
Absorption Spectrum ◽  
Effective Interaction ◽  
Coupling Reaction ◽  
Crystallographic Analysis ◽  
Synthesis And Characterization ◽  
X Ray ◽  
H Nmr ◽  
Cis Isomer ◽  
C Nmr

A unique class of azo porphyrin, 5,10,15,20-tetraphenyl-21-phenylazo-(2-aza-21-carbaporphyrin 1, in which an azophenyl group is embedded in N -confused porphyrin, was synthesized and characterized by 1 H NMR, 13 C NMR, UV-vis absorption, MS, and X-ray crystallographic analysis. Synthesis of 1 was achieved through a coupling reaction of 21-amino N -confused tetraphenylporphyrin with nitrosobenzene and subsequent deoxygenation of resulting azoxy derivative with a trioxo rhenium(VII) N -fused porphyrinato catalyst. The azo-conjugate molecule was exclusively obtained as a trans-isomer and no isomerization to the cis-isomer was observed under thermal or photoirradiation. The absorption spectrum of 1 shows a moderate red-shift due to the effective interaction between the porphyrinic π-system and the connecting azophenyl group. Upon protonation, this effect is essentially lost as a result of removing degeneracy of LUMO and LUMO+1.

scholarly journals Synthesis, Characterization, Crystal Structure, and Biological Studies of a Cadmium(II) Complex with a Tridentate Ligand 4′-Chloro-2,2′:6′,2′′-Terpyridine

2011 ◽  
Vol 2011 ◽  
pp. 1-7 ◽  
Author(s):  
L. A. Saghatforoush ◽  
L. Valencia ◽  
F. Chalabian ◽  
Sh. Ghammamy
Keyword(s):  
Crystal Structure ◽  
Ir Spectroscopy ◽  
Single Crystal ◽  
Antibacterial Activities ◽  
Tridentate Ligand ◽  
Single Crystal Diffraction ◽  
X Ray ◽  
H Nmr ◽  
Biological Studies ◽  
C Nmr

A new Cd(II) complex with the ligand 4′-chloro-2,2′6′,2′′-terpyridine (Cltpy), [Cd(Cltpy)(I)2], has been synthesized and characterized by CHN elemental analysis,1H-NMR,13C-NMR, and IR spectroscopy and structurally analyzed by X-ray single-crystal diffraction. The single-crystal X-ray analyses show that the coordination number in complex is five with three terpyridine (Cltpy) N-donor atoms and two iodine atoms. The antibacterial activities of Cltpy and its Cd(II) complex are tested against different bacteria.

Synthesis and Crystal Structure of Ocotillol-Type Metabolites Derived from (20R)-Protopanaxadiol

2017 ◽  
Vol 41 (4) ◽  
pp. 216-220 ◽  
Author(s):  
Zhi Liu ◽  
Yangrong Xu ◽  
Xingsi An ◽  
Jingjing Yang ◽  
Qingguo Meng ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Single Crystal Diffraction ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
H Nmr ◽  
The Absolute ◽  
C Nmr

Four ocotillol-type (20R)-protopanaxadiol metabolites, (20R,24S)-20,24-epoxy-12β,25-dihydroxdammaran-3-one (M3), and (20R,24R)-20,24-epoxy-12β,25-dihydroxydammarane-3-one (M4), (20R,24S)-20,24-epoxy-3β,25-dihydroxydammaran-12-one (M9) and (20R,24R)-20,24-epoxy-3β,25-dihydroxydammaran-12-one (M10) are synthesised from (20R)-protopanaxadiol. Their structures are confirmed by HRMS, 1H NMR and 13C NMR. Moreover, the absolute configurations of M3 and M4 are confirmed by the X-ray single crystal diffraction.

scholarly journals Synthesis and characterization of π–extended “earring” subporphyrins

2018 ◽  
Vol 14 ◽  
pp. 1956-1960 ◽  
Author(s):  
Haiyan Guan ◽  
Mingbo Zhou ◽  
Bangshao Yin ◽  
Ling Xu ◽  
Jianxin Song
Keyword(s):  
Single Crystal ◽  
Aromatic Ring ◽  
Nmr Spectra ◽  
Ring Current ◽  
Synthesis And Characterization ◽  
Single Crystal Diffraction ◽  
X Ray ◽  
H Nmr ◽  
Single Crystal Structures

A π-extended “earring” subporphyrin 3 was synthesized from β,β′-diiodosubporphyrin and diboryltripyrrane via a Suzuki–Miyaura coupling and following oxidation. Its Pd complex 3Pd was also synthesized and both of the compounds were fully characterized by 1H NMR, MS and X-ray single crystal diffraction. The 1H NMR spectra and single crystal structures revealed that aromatic ring current did not extend to the “ear” in both of the two compounds. Their UV–vis/NIR spectra were recorded and the absorption of both compounds is extended to the NIR region and that the absorption of 3Pd is further red-shifted and more intense.

scholarly journals Novel Synthesis and Characterization of Thiosemicarbazone Compounds Containing 4-Acyl-2-pyrazolin-5-ones

2009 ◽  
Vol 6 (3) ◽  
pp. 747-752 ◽  
Author(s):  
Arjun K. Rana ◽  
Nayan R. Parekh ◽  
Harish R. Dabhi ◽  
Sunil S. Nadkarni
Keyword(s):  
Free Radical Scavenger ◽  
Synthesis And Characterization ◽  
Radical Scavenger ◽  
Antibacterial And Antifungal Activity ◽  
X Ray ◽  
H Nmr ◽  
Novel Synthesis ◽  
Antibacterial And Antifungal ◽  
C Nmr

A novel synthesis of 4-acylthiosemicarbazone-3-methyl-1-(4`-methylphenyl)-2-pyrazolin-5-one by condensation of 4-acyl-3-methyl-1-(4`-methylphenyl)-2-pyrazolin-5-one with thiosemicarbazide is carried out. The compounds were characterized on the basis of elemental analysis, IR,1H NMR, Mass, DSC and13C NMR spectral data. The structures were investigated for their antibacterial and antifungal activity. They are very essential to study on cerebral infarction (Free radical scavenger). A single crystal X-ray study of this thiosemicarbazones and their metal complexes is in progress.

Design, synthesis, and herbicidal activity of novel 2-(arylamino)-5-methyl-4-methylene-7-(methylthio)-4H-pyrido[4,3-d][1,3]oxazine-8-carbonitrile derivatives

2019 ◽  
Vol 43 (3-4) ◽  
pp. 119-123
Author(s):  
Yi Sun ◽  
Wenfei Huang ◽  
Zhiqiang Li ◽  
Tao Wang ◽  
Jin Luo
Keyword(s):  
High Resolution Mass Spectrometry ◽  
Herbicidal Activity ◽  
Inhibition Rate ◽  
Target Compound ◽  
Single Crystal Diffraction ◽  
Design Synthesis ◽  
X Ray ◽  
H Nmr ◽  
Dicotyledonous Plants ◽  
C Nmr

A series of 5-methyl-4-methylene-7-methylthio-2-arylmino-4 H-pyrido[4,3- d][1,3]oxazine-8-carbonitrile derivatives were synthesized via tandem aza-Wittig and annulation reactions with { N-[3-acetyl-5-cyano-2-methyl-6-(methylthio)pyridin-4-yl]imino}triphenylphosphorane and aryl isocyanate in dry dichloromethane. Their structures were clearly confirmed by infrared, 1H NMR, 13C NMR, high-resolution mass spectrometry, and X-ray single-crystal diffraction. All newly synthesized compounds were screened for herbicidal activities against monocotyledonous and dicotyledonous plants. The results indicated that the target compound 2-[(4-methoxyphenyl)amino]-5-methyl-4-methylene-7-(methylthio)-4 H-pyrido[4,3- d][1,3]oxazine-8-carbonitrile showed 100% inhibition rate to grain sorghum (monocotyledonous) at the concentration of 100 mg L−1.

scholarly journals Environmentally Friendly Nafion-Catalyzed Synthesis of Substituted 2-Ethyl-3-Methylquinolines from Aniline and Propionaldehyde under Microwave Irradiation

Catalysts ◽  
2021 ◽  
Vol 11 (8) ◽  
pp. 877
Author(s):  
Chieh-Kai Chan ◽  
Chien-Yu Lai ◽  
Cheng-Chung Wang
Keyword(s):  
Reaction Mechanism ◽  
Microwave Irradiation ◽  
Single Crystal ◽  
Diffraction Analysis ◽  
Environmentally Friendly ◽  
Single Crystal Diffraction ◽  
X Ray ◽  
Related Data ◽  
Heating Source ◽  
Chemical Structures

Herein, we report a facile synthetic methodology for the preparation of 2,3-dialkylquinolines from anilines and propionaldehydes. This cyclization involved environmentally friendly Nafion® NR50 as an acidic catalyst with microwave irradiation as the heating source. A series of substituted 2-ethyl-3-methylquinolines were prepared from various anilines and propionaldehyde derivatives through this protocol with good to excellent yields. Some new chemical structures were confirmed by X-ray single-crystal diffraction analysis and the related data were provided. The plausible reaction mechanism studies are also discussed.

Ultrasound-assisted aqua-mediated synthesis of multi-substituted tetrahydropyridine-3-carboxylates using N-carboxymethyl-3-pyridinium hydrogensulfate ([N-CH2CO2H-3-pic]+HSO4−) as a new efficient ionic liquid catalyst

2021 ◽  
Vol 3 (6) ◽  
Author(s):  
Kobra Nikoofar ◽  
Fatemeh Shahriyari
Keyword(s):  
Ionic Liquid ◽  
Reaction Times ◽  
Aromatic Aldehydes ◽  
Environmentally Benign ◽  
H Nmr ◽  
Sonic Waves ◽  
Ft Ir ◽  
High Yields ◽  
Work Up ◽  
C Nmr

AbstractA simple, straightforward, and ultrasound-promoted method for the preparation of some highly functionalized tetrahydropyridines reported via pseudo five-component reaction of (hetero)aromatic aldehydes, different anilines, and alkyl acetoacetates in the presence of [N-CH2CO2H-3-pic]+HSO4−, as a novel ionic liquid, in green aqueous medium. The IL was synthesized utilizing simple and easily-handled substrates and characterized by FT-IR, 1H NMR, 13C NMR, GC-MASS, FESEM, EDX, and TGA/DTG techniques. The procedure contains some highlighted aspects which are: (a) performing the MCR in the presence of aqua and sonic waves, as two main important and environmentally benign indexes in green and economic chemistry, (b) high yields of products within short reaction times, (c) convenient work-up procedure, (d) preparing the new IL via simple substrates and procedure.

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