The Preparation of 1,2-Bis(2,2′:6′,2′′-Terpyridin-4′yl)Ethanone: The First Example of 4′-Terpyridyls Unsymmetrically Linked by a Functionalized Two-Carbon Chain

2004 ◽  
Vol 57 (7) ◽  
pp. 689 ◽  
Author(s):  
Zhi-Long Chen ◽  
Ronald N. Warrener ◽  
Douglas N. Butler
Keyword(s):  
Sulfuric Acid ◽  
Hydrochloric Acid ◽  
Single Crystal ◽  
Coupling Reaction ◽  
Carbon Chain ◽  
Sodium Cyanide ◽  
Starting Material ◽  
X Ray ◽  
Concentrated Sulfuric Acid ◽  
Single Crystal Analysis

1,2-Bis(2,2′:6′,2′′-terpyridin-4′yl)ethanone 7, an unsymmetrically linked bis-tridentatate ligand, was prepared by treatment of 4′-cyanomethylterpyridine 10 (RT, overnight) or 4′-(methoxycarbonylmethyl)terpyridine 11 (60°C, 7 h) with concentrated hydrochloric acid. These conversions, which involved an unprecedented homo-coupling reaction, are discussed with the structure of 7 being confirmed by X-ray single crystal analysis. The nitrile starting material 10 was prepared by reaction of the mesylate 9, derived from the known 4′-hydroxymethylterpyridine 8 with sodium cyanide, while ester 11 was prepared by reaction of 10 with methanol in the presence of concentrated sulfuric acid.

scholarly journals Stereoselective Convergent Synthesis of Carbon Skeleton of Cotylenin A Aglycone

Synthesis ◽  
2021 ◽  
Author(s):  
Kazuyuki Sugita ◽  
Motoi Kuwabara ◽  
Ami Matsuo ◽  
Shogo Kamo ◽  
Akinobu Matsuzawa
Keyword(s):  
Single Crystal ◽  
Aldol Reaction ◽  
Coupling Reaction ◽  
Carbon Skeleton ◽  
Convergent Synthesis ◽  
X Ray ◽  
Related Compounds

AbstractIn this paper, the synthesis of the carbon skeleton of cotylenin A aglycone is described. The key reactions, including an intramolecular aldol reaction, an aldol coupling reaction, and a ring-closing meta­thesis, allow for the effective and stereoselective access to the carbon skeleton of cotylenin A aglycone. The stereochemistry was confirmed by single-crystal X-ray crystallographic analyses of related compounds.

scholarly journals PICKLING EXPERIMENTAL STUDY ON PREPARATION OF DIESEL OIL WITH PYROLYSIS OIL FROM WASTE RUBBER

2017 ◽  
Vol 1 ◽  
pp. 169
Author(s):  
Wang Lei ◽  
Wang Yun ◽  
Jin Jie
Keyword(s):  
Experimental Study ◽  
Sulfuric Acid ◽  
Hydrochloric Acid ◽  
Diesel Oil ◽  
Pyrolysis Oil ◽  
Waste Rubber ◽  
Pickling Process ◽  
Concentrated Sulfuric Acid ◽  
Better Than

The research has been done for removing asphaltene by pickling process of diesel oil from pyrolysis oil self-made by waste rubber in this paper, and the study showed that pickling effect of concentrated sulfuric acid was better than concentrated hydrochloric acid. The best pickling effect was found when the concentration of sulfuric acid was 18.4mol/L, acid to oil ratio, namely, the amount of concentration of sulfuric acid to the amount of diesel oil ratio, was 25%. This experiment proved that removing asphaltene by pickling process using concentrated sulfuric acid was remarkable.

The modulated structure of the calcium aluminate Ca6(AlO2)12·Bi2O3

2010 ◽  
Vol 66 (6) ◽  
pp. 585-593 ◽  
Author(s):  
O. Pérez ◽  
S. Malo ◽  
M. Hervieu
Keyword(s):  
Single Crystal ◽  
Calcium Aluminate ◽  
Three Dimensional ◽  
X Ray Diffraction ◽  
Electron Pairs ◽  
Modulated Structure ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Superspace Formalism ◽  
Single Crystal Analysis

Bismuth calcium aluminate, Bi2Ca6Al12O27, has been prepared as a ceramic and a single crystal. Analysis of reciprocal space using both electron and X-ray diffraction show an R-centred hexagonal unit cell: a = b = 17.3892 (4), c = 6.986 (1) Å. Additional weak reflections are observed; they require the introduction of a modulation wavevector q = 0.0453 (2)c* for indexing. The modulated structure has been solved using the superspace formalism [superspace group X\overline{3}(00\gamma)0]. A framework of corner-sharing AlO4 tetrahedra forms corrugated sixfold rings and uncommon triple rings. The Ca2+ cations exhibit an eightfold coordination sphere; edge-sharing CaO8 polyhedra form intertwinned zigzagging rows along c creating a three-dimensional net. Bi atoms are located in large hexagonal tunnels parallel to c and form Bi2O3 pairs, which adopt a trigonal bipyramidal configuration. The 6s 2 lone-electron pairs (Lp) point along c, in the opposite direction to the three Bi—O strong bonds to form two BiO3Lp tetrahedra with a common base. Different orientations of the Bi2O3Lp2 pairs, rotated by 60° around c, are observed. Their stacking modes in each of the hexagonal tunnels are described. The sequence of the stacking varies along c in each of the tunnels.

X-ray single crystal analysis of the phase transitions in NH4MnCl3. Some Mossbauer-X-ray spectra relations

1978 ◽  
Vol 19 (1) ◽  
pp. 123-130 ◽  
Author(s):  
J. D. Tornero ◽  
F. H. Cano ◽  
J. Payos ◽  
M. Martinez-Ripoll
Keyword(s):  
Phase Transitions ◽  
Single Crystal ◽  
X Ray ◽  
Single Crystal Analysis

scholarly journals X-Ray Single Crystal Analysis of Oligo(oxymethylene) Diacetates

1993 ◽  
Vol 25 (12) ◽  
pp. 1275-1281 ◽  
Author(s):  
Koichi Ute ◽  
Takehito Takahashi ◽  
Ken-ichi Matsui ◽  
Koichi Hatada
Keyword(s):  
Single Crystal ◽  
X Ray ◽  
Single Crystal Analysis

scholarly journals Redetermination of ammonium metavanadate

IUCrData ◽  
2018 ◽  
Vol 3 (8) ◽  
Author(s):  
Aarón Pérez-Benítez ◽  
Sylvain Bernès
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonding ◽  
Solid State ◽  
Single Crystal ◽  
Structural Data ◽  
Ammonium Cation ◽  
Ammonium Metavanadate ◽  
Starting Material ◽  
X Ray ◽  
Hydrogen Bonding Interactions

The crystal structure of ammonium metavanadate, NH4VO3, a compound widely used as a starting material for the synthesis of vanadium and polyoxidovanadate compounds, had been determined twice using single-crystal X-ray data [Syneček & Hanic (1954). Czech. J. Phys. 4, 120–129 (Weissenberg data); Hawthorne & Calvo (1977). J. Solid State Chem. 22, 157–170 (four-circle diffractometer data)]. Its structure is now redetermined at higher resolution using Ag Kα radiation, and the result is compared with the former refinements. Structural data for the polymeric [VO3]∞ chain remain unchanged, while more accurate parameters are obtained for the ammonium cation, improving the description of hydrogen-bonding interactions in the crystal structure.

scholarly journals Facile Synthesis of 3-(Azol-1-yl)-1-adamantanecarboxylic Acids—New Bifunctional Angle-Shaped Building Blocks for Coordination Polymers

Molecules ◽  
2019 ◽  
Vol 24 (15) ◽  
pp. 2717 ◽  
Author(s):  
Dmitry Pavlov ◽  
Taisiya Sukhikh ◽  
Evgeny Filatov ◽  
Andrei Potapov
Keyword(s):  
Sulfuric Acid ◽  
Carboxylic Acid ◽  
Coordination Polymers ◽  
Building Blocks ◽  
X Ray Diffraction ◽  
Facile Synthesis ◽  
X Ray ◽  
Adamantanecarboxylic Acid ◽  
Concentrated Sulfuric Acid ◽  
First Time

For the first time, orthogonally substituted azole-carboxylate adamantane ligands were synthesized and used for preparation of coordination polymers. The angle-shaped ligands were prepared by the reaction of 1-adamantanecarboxylic acid and azoles (1H-1,2,4-triazole, 3-methyl-1H-1,2,4-triazole, 3,5-dimethyl-1H-1,2,4-triazole, 1H-tetrazole, 5-methyl-1H-tetrazole) in concentrated sulfuric acid. Variation of the solvent and substituents in azole rings allowed to prepare both 1D and 2D copper(II) and nickel(II) coordination polymers, [Cu2(trzadc)4(H2O)0.7]∙DMF∙0.3H2O, [Cu(trzadc)2(MeOH)]∙MeOH, [Ni(trzadc)2(MeOH)2] and [Cu2(mtrzadc)3(MeOH)]+NO3– (trzadc-3-(1,2,4-triazol-1-yl)-adamantane-1-carboxylic acid; mtrzadc-3-(3-methyl-1,2,4-triazol-1-yl)-adamantane-1-carboxylic acid) which were structurally characterized by single crystal X-ray diffraction. Complex [Cu(trzadc)2(MeOH)]∙MeOH was shown to act as a catalyst in the Chan-Evans-Lam arylation reaction.

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