Depsidone synthesis. XXIII. The oxidation of 2,2'-dihydroxy-4,4'-dimethoxy-6,6'-dimethylbenzophenone

1982 ◽  
Vol 35 (5) ◽  
pp. 1065 ◽  
Author(s):  
T Sala ◽  
MV Sargent ◽  
BW Skelton ◽  
AH White

Oxidation of 2,2'-dihydroxy-4,4'-dimethoxy-6,6'-dimethylbenzophenone (1) with alkaline ferricyanide gave the expected 4',6-dimethoxy-4,6'-dimethylspiro[benzofuran-2(3H),1'-cyclohexa-3',5'-diene]-2',3(2H)-dione (2) as well as 2'-hydroxy-6-methoxy-4,5'-dimethylspiro[benzofuran-2(3H),1'-cyclopent-4'-ene]-3(2H),3'-dione (3). The structure of compound (3) was deduced from its spectroscopic properties and was confirmed by X-ray diffraction.

2013 ◽  
Vol 66 (11) ◽  
pp. 1447 ◽  
Author(s):  
James E. M. Lewis ◽  
James D. Crowley

A series of copper(ii) complexes of the ligand 2,6-bis(pyridin-3-ylethynyl)pyridine have been synthesised and characterised by 1H and DOSY NMR, IR and UV-Vis spectroscopies, mass spectrometry, elemental analysis and single crystal X-ray diffraction. In solution these systems display almost identical spectroscopic properties, however the solid state structures are shown to vary widely, depending upon the choice of anion. The tetrafluoroborate salt was revealed to be a discrete Cu2L4 cage-like helicate. The tosylate salt, whilst of the same Cu2L4 stoichiometry, was shown to be a coordination polymer. Finally the nitrate salt structure was observed to be a discrete Cu2L2 metallocycle.


2003 ◽  
Vol 42 (19) ◽  
pp. 6024-6031 ◽  
Author(s):  
Vladimir B. Arion ◽  
Erwin Reisner ◽  
Madeleine Fremuth ◽  
Michael A. Jakupec ◽  
Bernhard K. Keppler ◽  
...  

2016 ◽  
Vol 71 (8) ◽  
pp. 909-917 ◽  
Author(s):  
Jia-Ming Li ◽  
Kun-Huan He ◽  
Zhong-Feng Shi ◽  
Hui-Yuan Gao ◽  
Yi-Min Jiang

AbstractTwo new metal-organic frameworks, namely, [Cd(L)(H2O)]n (1) and {[Cd0.5(L)(4,4′-bipy)0.5][Cd0.5(H2O)(4,4′-bipy)0.5]·H2O}n (2), where H2L = N-pyrazinesulfonyl-glycine and 4,4′-bipy = 4,4′-bipyridine, have been synthesized and characterized by single-crystal X-ray diffraction, IR spectroscopy, elemental, thermogravimetric, and photoluminescent analysis. X-ray diffraction crystallographic analyses indicate that 1 displays a distorted octahedral metal coordination in a 3-connected (4, 82) topology, while the molecular structure of 2 has a 4-connected (4, 4) topology with two perfectly octahedrally coordinated Cd centers. The L2– ligand serves as a N,N,O-tridentate, μ2-pyrazine-bridging, and μ2-carboxylate-bridging ligand in 1, and as a N,O-bidentate and μ2-carboxylate-bridging ligand in 2. In the crystal, a 3D supramolecular architecture is formed by O–H···O hydrogen bond interactions in 1, but through O–H···O as well as π···π stacking in 2. The two compounds show intense fluorescence in the solid state at room temperature.


1980 ◽  
Vol 33 (5) ◽  
pp. 1073 ◽  
Author(s):  
J Cannon ◽  
V Lojanapiwatna ◽  
C Raston ◽  
W Sinchai ◽  
A White

Plumbagin (1), droserone (2), hydroxydroserone (4) and four new quinones, nepenthone-A, nepenth-one-B, nepenthone-C (17) and nepenthone-E (9), have been isolated from the roots of Nepenthes rafflesiana Jack. A fifth quinone-nepenthone-D-has been detected in the extract and has been assigned the tentative structure (29) from its spectroscopic properties. ��� The crystal structure of nepenthone-E (9) was determined by X-ray diffraction; diffractometer data at 295 K were refined by full-matrix least squares to a residual of 0.061 (1040 'observed' reflections). Crystals of nepenthone-E (9) are triclinic, Pī a 7.579 (4), b 7.764 (5), c 10.806 (7) Ǻ, α 70.86 (4), β 101.40 (5), γ 91.70 (5)°, Z 2. ��� The structure of nepenthone-C (17) has been confirmed by an unambiguous synthesis. A synthesis of 2,7,8-trimethoxy-3-methyl-5,6-methylenedioxynaphtho-1,4-quinone (49) has revealed that this substance (49) is not identical with the O,O-dimethyl ether of nepenthone-A, and it is suggested that nepenthone-A is either the 5- or 8-O-methyl ether of 2,5,8-trihydroxy-3-methyl-6,7-methylenedioxy-naphtho-1,4-quinone [(36) or (37), respectively].


2016 ◽  
Vol 72 (4) ◽  
pp. 341-345 ◽  
Author(s):  
E. V. Bartashevich ◽  
V. I. Batalov ◽  
I. D. Yushina ◽  
A. I. Stash ◽  
Y. S. Chen

Two kinds of iodine–iodine halogen bonds are the focus of our attention in the crystal structure of the title salt, C12H8ClINO+·I3−, described by X-ray diffraction. The first kind is a halogen bond, reinforced by charges, between the I atom of the heterocyclic cation and the triiodide anion. The second kind is the rare case of a halogen bond between the terminal atoms of neighbouring triiodide anions. The influence of relatively weakly bound iodine inside an asymmetric triiodide anion on the thermal and Raman spectroscopic properties has been demonstrated.


1985 ◽  
Vol 38 (5) ◽  
pp. 809 ◽  
Author(s):  
H Becker ◽  
L Hansen ◽  
BW Skelton ◽  
AH White

(E)-1-(9-Anthryl)-2-(10-methyl-9-anthryl) ethelle has been synthesized from 10-methyl-9-anthraldehyde and (9-anthrylmethyl) triphenylphosphonium bromide, and its crystal structure has been determined by X-ray diffraction. Its molecular geometry was found to be such as to have the planes of the two anthracene moieties form an angle of 70.8°, the plane of the ethene bond bring twisted out of the planes of the anthracenes by an angle of about 55°. The intermolecular arrangement of parallel adjacent molecules in the crystal lattice is characterized by shifts about the short and long axes of the anthracenes. The excimer-like crystal fluorescence is attributed to the interplanar distance of 3.5 Ǻ between anthracene π- systems in parallel adjacent molecules. Crystals are triclinic, Pī , a 12.95(1), b 9.316(6), c 9.098(9) Ǻ, α 86.17(7), β 72.26(7), γ 74.61(6)°,Z 2; R was 0.054 for 1059 independent 'observed' reflections.


2011 ◽  
Vol 2011 ◽  
pp. 1-6 ◽  
Author(s):  
R. M. Ahmed ◽  
S. M. El-Bashir

FullereneC60has stimulated intense interest for scientific, industrial, and medical community because of its unique structure and properties. In the present study we prepared fullerene-doped nanocomposite films based on PMMA, PVAc, and PMMA/PVAc blend. Observations made by transmission electron microscope (TEM) showed the uniform dispersion ofC60nanoparticles in the polymer matrices. Also, X-ray diffraction measurements indicated thatC60has a tendency to form crystallites in the polymer matrices. In addition, the concentration effect of fullereneC60was investigated using optical absorption and photoluminescence spectroscopy. The spectroscopic properties of such films recommended their application in photonics and solar energy conversion.


Author(s):  
Hector Mario Heras Martinez ◽  
David Chavez Flores ◽  
Patrick C. Hillesheim ◽  
Siddappa Patil ◽  
Alejandro Bugarin

The title compound (E)-1,3-dimethyl-2-[3-(4-nitrophenyl)triaz-2-enylidene]-2,3-dihydro-1H-imidazole, C11H12N6O2, has monoclinic (C2/c) symmetry at 100 K. This triazene derivative was synthesized by the coupling reaction of 1,3-dimethylimidazolium iodide with 1-azido-4-nitro benzene in the presence of sodium hydride (60% in mineral oil) and characterized by 1H NMR, 13C NMR, IR, mass spectrometry, and single-crystal X-ray diffraction. The molecule consists of six-membered and five-membered rings, which are connected by a triazene moiety (–N=N—N–). In the solid-state, the molecule is found to be planar due to conjugation throughout the molecule. The extended structure shows two layers of molecules, which present weak intermolecular interactions that facilitate the stacked arrangement of the molecules forming the extended structure. Furthermore, there are several weak pseudo-cyclical interactions between the nitro oxygen atoms and symmetry-adjacent H atoms, which help to arrange the molecules.


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