scholarly journals Electrochemical generation of a catalyst for Michael addition of dicarbonyl compounds and cyanide anion to acryloylferrocene

2015 ◽  
Vol 13 (2) ◽  
pp. 67-76 ◽  
Author(s):  
Dragana Stevanovic ◽  
Anka Pejovic ◽  
Ivan Damljanovic ◽  
Mirjana Vukicevic ◽  
Sladjana Novakovic ◽  
...  
Keyword(s):  
Single Crystal ◽  
13C Nmr ◽  
Michael Addition ◽  
Ethyl Acetoacetate ◽  
Diethyl Malonate ◽  
1H And 13C Nmr ◽  
Electrochemical Generation ◽  
X Ray ◽  
Cyanide Anion

Michael addition of diethyl malonate, ethyl acetoacetate, acetylacetone, and cyanide anion to acryloylferrocene promoted by a catalyst in situ generated from a sacrificial zirconium anode is described. Most of the obtained compounds were identified by comparison of their spectral and physical data with those published elsewhere, whereas the only newly synthesized compound - diethyl 2,2-bis(3-ferrocenyl-3-oxopropyl)malonate - was completely characterized by spectral (IR, 1H- and 13C-NMR), physical and crystallographic (single-crystal X-ray) data.

scholarly journals Synthesis, characterization and crystal structure of butyl N-(3-chloropropyl)-(2S)-alaninate hydrochloride

2013 ◽  
Vol 78 (10) ◽  
pp. 1531-1537
Author(s):  
Dejana Dimitrijevic ◽  
Sladjana Novakovic ◽  
Gordana Radic ◽  
Verica Jevtic ◽  
Laura Menéndez-Taboada ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Nmr Spectroscopy ◽  
Single Crystal ◽  
Elemental Analysis ◽  
13C Nmr ◽  
13C Nmr Spectroscopy ◽  
1H And 13C Nmr ◽  
X Ray

The synthesis of butyl N-(3-chloropropyl)-(2S)-alaninate hydrochloride is reported here. The compound was characterized by elemental analysis, infrared, 1H and 13C NMR spectroscopy. The structure of butyl N-(3-chloropropyl)-(2S)-alaninate hydrochloride was confirmed by single-crystal X-ray analysis.

Single Crystal Growth of High-Pressure Phases of Ice and Salt Hydrate Far Below the Original Melting Point by Mixing Alcohol: Crystal Structure Determination of Magnesium Chloride Heptahydrate

2020 ◽  
Author(s):  
Keishiro Yamashita ◽  
Kazuki Komatsu ◽  
Hiroyuki Kagi
Keyword(s):  
Crystal Structure ◽  
High Pressure ◽  
Crystal Growth ◽  
Single Crystal ◽  
Room Temperature ◽  
Growth Technique ◽  
Salt Hydrate ◽  
X Ray

An crystal-growth technique for single crystal x-ray structure analysis of high-pressure forms of hydrogen-bonded crystals is proposed. We used alcohol mixture (methanol: ethanol = 4:1 in volumetric ratio), which is a widely used pressure transmitting medium, inhibiting the nucleation and growth of unwanted crystals. In this paper, two kinds of single crystals which have not been obtained using a conventional experimental technique were obtained using this technique: ice VI at 1.99 GPa and MgCl<sub>2</sub>·7H<sub>2</sub>O at 2.50 GPa at room temperature. Here we first report the crystal structure of MgCl2·7H2O. This technique simultaneously meets the requirement of hydrostaticity for high-pressure experiments and has feasibility for further in-situ measurements.

scholarly journals Tuning π-Acceptor/σ-Donor Ratio of the 2-Isocyanoazulene Ligand: Non-Fluorinated Rival of Pentafluorophenyl Isocyanide and Trifluorovinyl Isocyanide Discovered

Molecules ◽  
2021 ◽  
Vol 26 (4) ◽  
pp. 981
Author(s):  
Mason D. Hart ◽  
John J. Meyers ◽  
Zachary A. Wood ◽  
Toshinori Nakakita ◽  
Jason C. Applegate ◽  
...  
Keyword(s):  
Charge Transfer ◽  
Coordination Chemistry ◽  
Single Crystal ◽  
13C Nmr ◽  
Quantitative Assessment ◽  
X Ray ◽  
New Class ◽  
Linear Relationships ◽  
Ligand Charge Transfer ◽  
Donor Characteristics

Isocyanoazulenes (CNAz) constitute a relatively new class of isocyanoarenes that offers rich structural and electronic diversification of the organic isocyanide ligand platform. This article considers a series of 2-isocyano-1,3-X2-azulene ligands (X = H, Me, CO2Et, Br, and CN) and the corresponding zero-valent complexes thereof, [(OC)5Cr(2-isocyano-1,3-X2-azulene)]. Air- and thermally stable, X-ray structurally characterized 2-isocyano-1,3-dimethylazulene may be viewed as a non-benzenoid aromatic congener of 2,6-dimethyphenyl isocyanide (2,6-xylyl isocyanide), a longtime “workhorse” aryl isocyanide ligand in coordination chemistry. Single crystal X-ray crystallographic {Cr–CNAz bond distances}, cyclic voltametric {E1/2(Cr0/1+)}, 13C NMR {δ(13CN), δ(13CO)}, UV-vis {dπ(Cr) → pπ*(CNAz) Metal-to-Ligand Charge Transfer}, and FTIR {νN≡C, νC≡O, kC≡O} analyses of the [(OC)5Cr(2-isocyano-1,3-X2-azulene)] complexes provided a multifaceted, quantitative assessment of the π-acceptor/σ-donor characteristics of the above five 2-isocyanoazulenes. In particular, the following inverse linear relationships were documented: δ(13COtrans) vs. δ(13CN), δ(13COcis) vs. δ(13CN), and δ(13COtrans) vs. kC≡O,trans force constant. Remarkably, the net electron withdrawing capability of the 2-isocyano-1,3-dicyanoazulene ligand rivals those of perfluorinated isocyanides CNC6F5 and CNC2F3.

In-situ X-ray tomography investigation of pore damage effects during a tensile test of a Ni-based single crystal superalloy

2021 ◽  
pp. 111180
Author(s):  
Keli Liu ◽  
Junsheng Wang ◽  
Bing Wang ◽  
Pengcheng Mao ◽  
Yanhong Yang ◽  
...  
Keyword(s):  
Tensile Test ◽  
Single Crystal ◽  
Single Crystal Superalloy ◽  
X Ray

Ultrasound-Promoted Synthesis of Spirocyclopropanes from Switchable Starting Materials via Azomethine Ylide [3+2]-Cycloaddition

Synthesis ◽  
2021 ◽  
Author(s):  
Issa Yavari ◽  
Sara Sheikhi ◽  
Jamil Sheykhahmadi ◽  
Zohreh Taheri ◽  
Mohammad Reza Halvagar
Keyword(s):  
Single Crystal ◽  
Azomethine Ylides ◽  
Azomethine Ylide ◽  
X Ray ◽  
Green Protocol ◽  
Stereogenic Centers ◽  
Quinoxaline Derivatives ◽  
Excellent Selectivity

AbstractAn ultrasound-promoted green protocol to access a new series of spirocyclopropanes from indeno[1,2-b]quinoxaline derivatives and azomethine ylides, generated in situ from the iodine-catalyzed reaction of acetophenones as well as of 2-methylquinoline with pyridine in the presence of a base, is described. These transformations proceed via a spirocyclopropanation reaction followed by elimination of pyridine. Clear evidence for the structure of a spirocyclopropane-linked indenoquinoxaline derivative was obtained from single-crystal X-ray analysis. The most important feature of this reaction is the fact it forms three stereogenic centers, one of which is quaternary, with excellent selectivity.

ChemInform Abstract: Structure of 4-Substituted 3,4′-Diquinolinyl Sulfides Studied by 1H and 13C NMR and X-Ray Analysis

ChemInform ◽  
2010 ◽  
Vol 24 (27) ◽  
pp. no-no
Author(s):  
A. MASLANKIEWICZ ◽  
M. WYSZOMIRSKI ◽  
S. BORYCZKA ◽  
A. GOGOLL ◽  
T. GLOWIAK
Keyword(s):  
13C Nmr ◽  
1H And 13C Nmr ◽  
X Ray ◽  
Abstract Structure
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