Synthesis of 2,3-Anhydro Glycosyl Phosphonates

1996 ◽  
Vol 49 (3) ◽  
pp. 371 ◽  
Author(s):  
m Doanxuanlie ◽  
ID Jenkins ◽  
BW Skelton ◽  
AH White
Keyword(s):  
Hydrogen Peroxide ◽  
Structural Analysis ◽  
Sodium Tungstate ◽  
X Ray

The synthesis of dimethyl 6-O-acetyl-2,3-anhydro-α-D- mannopyranosylphosphonates and the corresponding α- and β- allo derivatives is described. Dimethyl 4,6-di-O-acetyl-2,3-dideoxy-D-erythro-hex-2-enopyranosylphosphonates, although unreactive towards normal epoxidizing agents (3-chloroperoxybenzoic acid, trifluoroperoxyacetic acid, etc), underwent smooth epoxidation with hydrogen peroxide in the presence of sodium tungstate or dodecatungstophosphoric acid. An interesting regiospecific deacetylation of the 4-acetate occurred under these conditions. The structures of these anhydro glycosyl phosphonates were determined by 1H and 13C n.m.r. spectroscopy, and confirmed by X ray structural analysis in the case of dimethyl 6-O-acetyl-2,3-anhydro-α-D-mannopyranosylphosphonate , and of dimethyl 6-O-acetyl-2,3-anhydro-β-D-allopyranosylphosphonate.

scholarly journals Attempted Synthesis and Unexpected β-Fragmentation of a Hindered β-Keto Nitroxide

2017 ◽  
Vol 70 (10) ◽  
pp. 1106 ◽  
Author(s):  
Chris Edwards ◽  
Peter C. Healy ◽  
W. Ken Busfield ◽  
Ezio Rizzardo ◽  
San H. Thang ◽  
...  
Keyword(s):  
Hydrogen Peroxide ◽  
Ring Opening ◽  
Sodium Tungstate ◽  
Crystallographic Analysis ◽  
High Yield ◽  
Fragmentation Mechanism ◽  
Pentanoic Acid ◽  
X Ray ◽  
Ring Opening Reaction

The attempted synthesis of a β-keto imidazolidinone nitroxide by oxidation of the β-hydroxy imidazolidinone precursor with hydrogen peroxide and sodium tungstate led to an unexpected ring-opening reaction to produce 1,4-diazaspiro[4.5]dec-1-en-3-oxo-2-pentanoic acid 1-oxide (13) in high yield. The structure of 13 was confirmed by X-ray crystallographic analysis. A β-fragmentation mechanism is suggested for the oxidative ring-opening reaction.

RNA polymerase: Preparation and structural analysis of helical polymers

1984 ◽  
Vol 42 ◽  
pp. 152-153
Author(s):  
E. Loren Buhle ◽  
Pamela Rew ◽  
Ueli Aebi
Keyword(s):  
Structural Analysis ◽  
Rna Polymerase ◽  
Molecular Level ◽  
X Ray Diffraction ◽  
Helical Polymers ◽  
X Ray ◽  
E Coli ◽  
The Past ◽  
Ordered Arrays ◽  
Low Ionic Strength

While DNA-dependent RNA polymerase represents one of the key enzymes involved in transcription and ultimately in gene expression in procaryotic and eucaryotic cells, little progress has been made towards elucidation of its 3-D structure at the molecular level over the past few years. This is mainly because to date no 3-D crystals suitable for X-ray diffraction analysis have been obtained with this rather large (MW ~500 kd) multi-subunit (α2ββ'ζ). As an alternative, we have been trying to form ordered arrays of RNA polymerase from E. coli suitable for structural analysis in the electron microscope combined with image processing. Here we report about helical polymers induced from holoenzyme (α2ββ'ζ) at low ionic strength with 5-7 mM MnCl2 (see Fig. 1a). The presence of the ζ-subunit (MW 86 kd) is required to form these polymers, since the core enzyme (α2ββ') does fail to assemble into such structures under these conditions.

Heterogeneous Fenton Catalytic Removal of Organic Pollutant in Aqueous Solution by using Coal Gangue as a Catalyst

2019 ◽  
Vol 12 (4) ◽  
pp. 312-325
Author(s):  
Jiwei Zhang ◽  
Jingjing Xu ◽  
Shuaixia Liu ◽  
Baoxiang Gu ◽  
Feng Chen ◽  
...  
Keyword(s):  
Aqueous Solution ◽  
Hydrogen Peroxide ◽  
Hydroxyl Radical ◽  
Removal Rate ◽  
Organic Pollutant ◽  
Coal Gangue ◽  
Ion Leakage ◽  
Heterogeneous Fenton ◽  
Solution Ph ◽  
X Ray

Background: Coal gangue was used as a catalyst in heterogeneous Fenton process for the degradation of azo dye and phenol. The influencing factors, such as solution pH gangue concentration and hydrogen peroxide dosage were investigated, and the reaction mechanism between coal gangue and hydrogen peroxide was also discussed. Methods: Experimental results showed that coal gangue has the ability to activate hydrogen peroxide to degrade environmental pollutants in aqueous solution. Under optimal conditions, after 60 minutes of treatment, more than 90.57% of reactive red dye was removed, and the removal efficiency of Chemical Oxygen Demand (COD) up to 72.83%. Results: Both hydroxyl radical and superoxide radical anion participated in the degradation of organic pollutant but hydroxyl radical predominated. Stability tests for coal gangue were also carried out via the continuous degradation experiment and ion leakage analysis. After five times continuous degradation, dye removal rate decreased slightly and the leached Fe was still at very low level (2.24-3.02 mg L-1). The results of Scanning Electron Microscope (SEM), energy dispersive X-Ray Spectrometer (EDS) and X-Ray Powder Diffraction (XRD) indicated that coal gangue catalyst is stable after five times continuous reuse. Conclusion: The progress in this research suggested that coal gangue is a potential nature catalyst for the efficient degradation of organic pollutant in water and wastewater via the Fenton reaction.

The crystal and molecular structure of tris(pentamethylenedithiocarbamate) chromium(III)-chloroform (1 : 2)

1981 ◽  
Vol 46 (1) ◽  
pp. 6-19 ◽  
Author(s):  
Viktor Kettman ◽  
Ján Garaj ◽  
Jaroslav Majer
Keyword(s):  
Molecular Structure ◽  
Structural Analysis ◽  
Crystal And Molecular Structure ◽  
Analysis Method ◽  
Complex Molecules ◽  
Coordination Polyhedra ◽  
X Ray ◽  
Cell Dimensions ◽  
Crustal Density ◽  
Unit Cell Dimensions

The crystal and molecular structure of [Cr(S2CN(CH2)5)3].2 CHCl3 was found by the X-ray structural analysis method. The value R 0.090 was found for 1 131 observed independent reflections. The substance crystallizes in a space group of symmetry P212121 with the following unit cell dimensions: a = 0.8675 (6), b = 1.815(2), c = 2.155(3) nm. The experimentally observed crustal density was 1.48 Mgm-3 and the value calculated for Z = 4 was 1.51 Mgm-3. The CrS6 coordination polyhedron has the shape of a trigonally distorted octahedron, where the D3 symmetry is a approximately retained. The degree of trigonal distortion expressed as the projection of the chelate S-Cr-S angle onto the plane perpendicular to the C3 pseudo axis is Φ = 41.7° (Φ = 60° for an octahedron). The skeleton of the structure formed by the complex molecules contains channels filled with chloroform molecules. The specific type of complex-chloroform interaction consists of the formation of hydrogen bonds of the chloroform protons with the fully occupied pπ-orbitals of the sulphur atoms in the coordination polyhedra. The low stability and crystal decomposition can be explained by loss of chloroform from the channels.

Reactivity of Sodium Hexaethyl-2,4-dicarba-nido-hexaborate(1-)

1999 ◽  
Vol 64 (6) ◽  
pp. 977-985 ◽  
Author(s):  
Bernd Wrackmeyer ◽  
Hans-Jörg Schanz ◽  
Wolfgang Milius ◽  
Catherine McCammon
Keyword(s):  
Mössbauer Spectroscopy ◽  
Nmr Spectroscopy ◽  
Structural Analysis ◽  
Hydrogen Atom ◽  
Mossbauer Spectroscopy ◽  
Sandwich Complex ◽  
X Ray ◽  
Bromo Derivative ◽  
Boron Tribromide ◽  
C Nmr

Sodium hexaethyl-2,4-dicarba-nido-hexaborate(1-) (6), available from hexaethyl-2,4-dicarba- nido-hexaborane(8) (4) by deprotonation, reacts with deuterated methanol, CD3OD, to give back 4 without H/D exchange of the B-H-B hydrogen atom. The reaction of 6 with diethylboron chloride, Et2BCl, affords hexaethyl-2,4-dicarba-closo-hexaborane(6) (7), the first example of a peralkylated carborane of this type. In contrast, the reaction of 6 with boron tribromide, BBr3, leads mainly to 2,3,4,5,6,7-hexaethyl-2,4-dicarba-closo-heptaborane(7) (8), together with the corresponding 1-bromo derivative (9) and the closo-carborane 7 as side products. The reaction of two equivalents of 6 with FeCl2 gives the air-stable sandwich complex bis[hexaethyl-2,4-dicarba-nido-hexaborate(1-)]iron 10 which was characterised by X-ray structural analysis. All products were characterised by 1H, 11B and 13C NMR spectroscopy, and 57Fe Mössbauer spectroscopy was used to study 10.

Crystal and solution structure of (E)-1,2-bis(ethylsulphonyl)cyclobutane-1,2-dicarbonitrile

1989 ◽  
Vol 54 (12) ◽  
pp. 3253-3259
Author(s):  
Jaroslav Podlaha ◽  
Miloš Buděšínský ◽  
Jana Podlahová ◽  
Jindřich Hašek
Keyword(s):  
Hydrogen Peroxide ◽  
Solution Structure ◽  
Peroxide Oxidation ◽  
X Ray ◽  
X Ray Crystallography ◽  
Nmr Study ◽  
Hydrogen Peroxide Oxidation ◽  
Unusual Product ◽  
C Nmr

The unusual product of the reaction of 2-chloroacrylonitrile with ethane thiol and following hydrogen peroxide oxidation was found to be (E)-1,2-bis(ethylsulphonyl)cyclobutane-1,2-dicarbonitrile by means of X-ray crystallography. 1H and 13C NMR study of this compound has proven the same conformation of the molecule in solution.

scholarly journals X-Ray Structural Analysis of Molten KF–KX(X=Cl, Br, and I) Systems

1987 ◽  
Vol 1987-7 (1) ◽  
pp. 165-174
Author(s):  
Yoshihiro OKAMOTO
Keyword(s):  
Structural Analysis ◽  
X Ray

scholarly journals Light-induced [2 + 2] Cycloaddition of 6-Methoxy-2-naphthonitrile to 2-Chloroacrylonitrile

1999 ◽  
Vol 23 (1) ◽  
pp. xiv-xiv
Author(s):  
Nader A. Al-Jalal ◽  
Robin G. Pritchard ◽  
Charles A. McAuliffe
Keyword(s):  
Structural Analysis ◽  
X Ray

6-Methoxy-2-naphthonitrile undergoes photocycloaddition to 2-chloroacrylonitrile to give [2 + 2] cyclobutane adducts (1a and 1b), the structure of one of which (1a) has been unambiguously confirmed by an X-ray structural analysis.

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