scholarly journals 2-Diphenylphosphinomethyl-3-methylpyrazine

Molbank ◽  
10.3390/m1267 ◽  
2021 ◽  
Vol 2021 (3) ◽  
pp. M1267
Author(s):  
Tiziana Boccuzzi ◽  
Luciana Cicco ◽  
Andrea Francesca Quivelli ◽  
Paola Vitale ◽  
Filippo Maria Perna ◽  
...  
Keyword(s):  
Magnetic Resonance ◽  
Single Crystals ◽  
Methyl Ether ◽  
Environmentally Friendly ◽  
Spectroscopic Techniques ◽  
X Ray ◽  
First Report ◽  
Moderate Yield ◽  
Type Intermediate ◽  
Multinuclear Magnetic Resonance

The lateral metalation-electrophilic trapping reaction of alkyl-substituted pyrazines has always been challenging and poorly regioselective, with the corresponding derivatives often being isolated in moderate yield. In this contribution, we first report on the preparation of an unsymmetrically-substituted pyrazine, that is 2-diphenylphosphinomethyl-3-methylpyrazine, by subjecting to metalation with n-BuLi the commercially available 2,3-dimethylpyrazine, followed by interception of the putative lithiated benzyl-type intermediate with Ph2PCl. Such a functionalization has been successfully carried out in the absence of additional ligands, working either in THF at −78 °C or in a more environmentally friendly solvent like cyclopentyl methyl ether at 0 °C, with the desired phosphine derivative being isolated in 70–85% yield. The newly synthesized adduct has been fully characterized by means of multinuclear magnetic resonance spectroscopic techniques, and also by preparing a selenium derivative, which furnished single crystals that were suitable for X-ray analysis.

Synthesis of 1,2,3-triazole-substituted 6,7-dihydroindolizin-8(5H)-one derivatives mediated by Selectfluor

2019 ◽  
Vol 43 (5-6) ◽  
pp. 179-183
Author(s):  
Yulin Huang ◽  
Jiaying Lei ◽  
Xinliang Fu ◽  
Wenlin Xie ◽  
Xiaofang Li
Keyword(s):  
Mass Spectrometry ◽  
Nuclear Magnetic Resonance ◽  
Magnetic Resonance ◽  
High Resolution ◽  
High Resolution Mass Spectrometry ◽  
Crystallographic Analysis ◽  
X Ray ◽  
High Resolution Mass ◽  
Moderate Yield ◽  
Resolution Mass

The 1,2,3-triazole and 1 H-1,2,3-benzotriazole-substituted 6,7-dihydroindolizin-8(5 H)-one derivatives were synthesized by the reaction of ( E)-7-(arylmethylidene)-6,7-dihydroindolizin-8(5 H)-ones with 1,2,3-triazole and 1 H-1,2,3-benzotriazole in the presence of Selectfluor in moderate yield. The structures of all the products were characterized thoroughly by nuclear magnetic resonance, infrared, and high-resolution mass spectrometry together with X-ray crystallographic analysis.

Alkyl chlorido hydridotris(3,5-dimethylpyrazolyl)borate imido niobium and tantalum(v) complexes: synthesis, conformational states of alkyl groups in solid and solution, X-ray diffraction and multinuclear magnetic resonance spectroscopy studies

2014 ◽  
Vol 43 (15) ◽  
pp. 5747-5758 ◽  
Author(s):  
Miguel Galájov ◽  
Carlos García ◽  
Manuel Gómez ◽  
Pilar Gómez-Sal
Keyword(s):  
Magnetic Resonance ◽  
Magnetic Resonance Spectroscopy ◽  
Resonance Spectroscopy ◽  
X Ray Diffraction ◽  
Conformational States ◽  
X Ray ◽  
Alkyl Groups ◽  
Spectroscopy Studies ◽  
Multinuclear Magnetic Resonance

A series of new alkyl imido hydridotris(3,5-dimethylpyrazolyl)borate niobium and tantalum complexes have been synthesized and characterized.

1,3,2-Diazaphospha-[3]ferrocenophanes. Molecular Structures and Multinuclear Magnetic Resonance Studies

2009 ◽  
Vol 64 (11-12) ◽  
pp. 1401-1412 ◽  
Author(s):  
Bernd Wrackmeyer ◽  
Elena V. Klimkina ◽  
Wolfgang Milius
Keyword(s):  
Molecular Structure ◽  
Solid State ◽  
Structural Analysis ◽  
Magnetic Resonance ◽  
Phosphorus Atom ◽  
Molecular Structures ◽  
Magnetic Resonance Studies ◽  
X Ray ◽  
Nmr Techniques ◽  
Multinuclear Magnetic Resonance

2-Phenoxy-1,3,2-diazaphospha-[3]ferrocenophane and related derivatives (oxide, sulfide, selenide) were prepared, characterized in solution by multinuclear magnetic resonance methods (1D and 2D 1H, 13C, 15N and 31P NMR) and in the solid state by X-ray structural analysis. The conformation of the 2-phenoxy derivative differs from that of the 2-tert-butyl compound. For further comparison, 2-R- 2,3-dihydro-1H-1,3,2-diazaphospha-phenalene derivatives R = 'Bu, PhO were prepared and studied by the same NMR techniques. The molecular structure of a selenide was determined, and together with the NMR evidence, it was concluded that the conformation of these heterocycles is independent of the respective substituent at the phosphorus atom

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