The two solid-state conformations of nefopam methiodide, a quaternary ammonium salt of the analgesic drug

1990 ◽  
Vol 68 (7) ◽  
pp. 1128-1134 ◽  
Author(s):  
Robert Glaser ◽  
André Michel ◽  
Marc Drouin
Keyword(s):  
Solid State ◽  
Ammonium Salt ◽  
Quaternary Ammonium ◽  
Quaternary Ammonium Salt ◽  
State Structure ◽  
X Ray Diffraction ◽  
Analgesic Drug ◽  
X Ray ◽  
Positional Disorder ◽  
X Ray Crystallography

The solid-state structure of nefopam methiodide, a quaternary ammonium salt of nefopam hydrochloride (a non-narcotic analgesic drug), has been determined by single crystal X-ray diffraction analysis. Nefopam methiodide gives crystals belonging to the monoclinic P21/c space group and, at 298 K, a = 10.001(1), b = 9.928(1), c = 17.598(1) Å, β = 94.41(1)°, V = 1742.2(2) Å3, Z = 4, R(F) = 0.086, and Rw(F) = 0.108. Due to disorder, the boat (flattened chair) and twist-chair (flattened chair) conformations of the 2,5-benzoxazocine eight-membered ring were both observed in the crystal with 55:45 occupancy, respectively. Positional disorder was also observed for the iodide counterion, which showed occupancies of 81:9.5:9.5. Keywords: nefopam, analgesic, X-ray crystallography, conformation.

scholarly journals Novel Enantiomerically Pure Ferrocenes

1996 ◽  
Vol 51 (3) ◽  
pp. 437-440 ◽  
Author(s):  
Adolphus A . H. van der Zeijden ◽  
J. Sieler ◽  
E. Hovestreydt
Keyword(s):  
Solid State ◽  
Ammonium Salt ◽  
State Structure ◽  
X Ray Diffraction ◽  
Dimethylamino Group ◽  
Enantiomerically Pure ◽  
Solid State Structure ◽  
X Ray ◽  
Cyclopentadienyl Ligand

Abstract A chiral ferrocene (CpE2Fe) was synthesized by reaction of CpELi with FeCl2(THF)1.5 The cyclopentadienyl ligand CpE contains a dimethylamino group that is separated from the Cp backbone by two stereogenic carbon centres. Reaction of CpE2Fe with excess Mel affords the ammonium salt CpE2Fe.2MeI. Its solid state structure was determined by X-ray diffraction methods.

Organophilization of Four Differents Bentonitic Clays with a Quaternary Ammonium Salt

2005 ◽  
Vol 498-499 ◽  
pp. 67-72 ◽  
Author(s):  
Daniela de Lourdes A.C.S. Andrade ◽  
Wildemberg A. Freire ◽  
Sueila S. Araújo ◽  
Lucianna G.F. Vieira ◽  
Ana Cristina Figueiredo de Melo Costa ◽  
...  
Keyword(s):  
Polymer Nanocomposites ◽  
Ammonium Salt ◽  
Quaternary Ammonium ◽  
Quaternary Ammonium Salt ◽  
Drilling Fluids ◽  
X Ray Diffraction ◽  
X Ray ◽  
Dimethyl Benzyl ◽  
Dimethyl Benzyl Ammonium ◽  
Petroleum Drilling

Organophilic Bentonities clays are widely used for industrial purposes, as components of petroleum drilling fluids as well as in cosmetics, lubricants adhesives and paints. Most recent they have been used as fillers in polymer nanocomposites. In this work, three organophilic bentonitic clays from the distric of Boa Vista and one from Campina Grande, PB, Brazil, were synthesized and characterized. The four clays were treated with a quaternary chloride ammonium salt- dimethyl benzyl ammonium alkyl chloride (Dodigen 1611) provided by Chemco. The cation exchange and swelling capacities of the modified clays were determined and the clays were characterized by FTIR, Thermal Analysis (DTA, TGA) and X-ray diffraction. The results showed the modification of all four clays by the quaternary ammonium salt to be successful.

Reversible phase transformation-type layer shape electrolyte based on POM and quaternary ammonium salt

2014 ◽  
Vol 07 (02) ◽  
pp. 1450019 ◽  
Author(s):  
Xuefei Wu ◽  
Yunyan Li ◽  
Qingyin Wu ◽  
Hong Ding ◽  
Wenfu Yan
Keyword(s):  
Ammonium Salt ◽  
Quaternary Ammonium ◽  
Quaternary Ammonium Salt ◽  
Water Solution ◽  
X Ray Diffraction ◽  
Inorganic Layer ◽  
X Ray ◽  
Type Layer ◽  
Transformation Type ◽  
Reversible Phase

A novel kind of organic–inorganic layer shape material, polyoxymetalates (POM)-type ionic liquid (IL) with Keggin structure and simple quaternary ammonium salt, (TOAMe)4PW11VO40 (trioctylmethylammonium = TOAMe,…) is synthesized and characterized by IR, UV, X-ray diffraction (XRD), TG–DTA. Its electrochemical property was investigated by cyclic voltammgram. Research results released the vanadium and the POM structure in the compound can process reduction in DMSO, which is unlikely in water solution as a simple hydrated ion because water will protonize substrate.

Identification of Phenothiazine Derivatives and Analogs by X-Ray Diffraction. II. Active Substances in Pharmaceutical Formulations

1971 ◽  
Vol 54 (3) ◽  
pp. 633-639
Author(s):  
A De Leenheer ◽  
A Heyndrickx
Keyword(s):  
Ammonium Salt ◽  
Quaternary Ammonium ◽  
Quaternary Ammonium Salt ◽  
Pharmaceutical Formulations ◽  
X Ray Diffraction ◽  
Phenothiazine Derivatives ◽  
X Ray ◽  
Diffraction Patterns ◽  
Related Compounds ◽  
Active Substances

Abstract Procedures have been developed for the isolation of phenothiazines and chemically related compounds from pharmaceutical formulations, namely, injections, solutions, tablets, coated tablets, creams, sirups, lotions, and suppositories. In general, active substances are crystallized as picrates. A few compounds, however, gave better crystalline derivatives as free bases (levomepromazine and propericiazine), quaternary ammonium salt (thiazinamium), or chlorhydrate salts (amitriptyline and nortriptyline). The crystalline derivatives prepared were specifically identified by comparison of their Debye-Scherrer X-ray diffraction patterns with those for reference compounds obtained under the same conditions.

Synthesis and structural characterization of a magnesium phthalocyanine(3–) anion

2012 ◽  
Vol 16 (01) ◽  
pp. 154-162 ◽  
Author(s):  
Edwin W.Y. Wong ◽  
Daniel B. Leznoff
Keyword(s):  
Absorption Spectrum ◽  
Solid State ◽  
Single Crystal ◽  
Structural Characterization ◽  
Heterometallic Complex ◽  
State Structure ◽  
Solid State Structure ◽  
X Ray ◽  
X Ray Crystallography

The reduction of magnesium phthalocyanine (MgPc) with 2.2 equivalents of potassium graphite in 1,2-dimethoxyethane (DME) gives [K2(DME)4]PcMg(OH)(1) in 67% yield. Compound 1 was structurally characterized using single crystal X-ray crystallography and was found to be a monomeric, heterometallic complex consisting of a μ3-OH ligand that bridges a [MgIIPc3-]- anion to two potassium cations solvated by four DME molecules. An absorption spectrum of 1 confirms the Pc ligand is singly reduced and has a 3–charge. The solid-state structure of 1 does not indicate breaking of the aromaticity of the Pc ligand. Compound 1 is only the second Pc3- complex and the first reduced MgPc to be isolated and structurally characterized.

Unprecedented Hexa- and Undecanuclear Frameworks of Two New Tin(IV) Oxo Clusters Resulting from Partial Debenzylation Reactions

2010 ◽  
Vol 65 (11) ◽  
pp. 1293-s1308 ◽  
Author(s):  
Laurent Plasseraud ◽  
Hélène Cattey ◽  
Philippe Richard
Keyword(s):  
Solid State ◽  
1H Nmr Spectroscopy ◽  
Trifluoromethanesulfonic Acid ◽  
Synthetic Route ◽  
State Structure ◽  
X Ray Diffraction ◽  
Neutral Cluster ◽  
Broad Resonance ◽  
X Ray ◽  
The Core

A new and facile synthetic route to the known neutral cluster ((PhCH2)2SnO)6[((PhCH2)2SnOH)2- (CO3)]2 (2) as well as its reactivity toward trifluoromethanesulfonic acid (HO3SCF3, TfOH) are reported. The solid-state structure of the new solvate 2·6C7H8 has been determined by single-crystal X-ray diffraction. The core of 2 can be described as a pair of coplanar pentanuclear [(PhCH2)2SnO]5 ladders bridged at their ends by two carbonate groups. Successive additions of TfOH to a suspension of 2 in CD3CN were monitored by 119Sn{1H} NMR spectroscopy showing the transformation of the fingerprint of 2 (δ = −244, −246, −306 ppm), via new upfield signals, to a final broad resonance located at δ = −474 ppm. Thereafter, two unprecedented ionic monobenzyltin(IV) oxo clusters, 3 and 4, resulting from a debenzylation reaction and exhibiting unusual hexa- and undecanuclear frameworks, respectively, have been isolated as single crystals.

N–O Bond Cleavage During the Deprotonation of N,O-Bis(trimethylsilyl)hydroxylamine

2008 ◽  
Vol 63 (3) ◽  
pp. 339-341 ◽  
Author(s):  
Ajay Venugopal ◽  
Alexander Willner ◽  
Norbert W. Mitzel
Keyword(s):  
Solid State ◽  
Single Crystal ◽  
Elemental Analysis ◽  
Bond Cleavage ◽  
State Structure ◽  
X Ray Diffraction ◽  
Solid State Structure ◽  
X Ray ◽  
Potassium Hydride ◽  
Oxygen Atoms

The reaction of N,O-bis(trimethylsilyl)hydroxylamine with potassium hydride in pentane affords a product of the formula {K6[OSiMe3]4[ON(SiMe3)2]2}, resulting from deprotonation followed by N-O bond cleavage and 1,2-silylshift. The compound was characterised by elemental analysis and by single crystal X-ray diffraction. The aggregate consists of a K3O3 bis-cubane core, with N(SiMe3)2 groups at the oxygen atoms shared by the two cubes, andMe3Si groups attached to the four O vertices. Two weak K···N interactions are also detected in the solid state structure.

Notizen: Solid State Structure of N,N-Dibenzylhydroxylamine

1995 ◽  
Vol 50 (4) ◽  
pp. 699-701 ◽  
Author(s):  
Norbert W. Mitzel ◽  
Jürgen Riede ◽  
Klaus Angermaier ◽  
Hubert Schmidbaur
Keyword(s):  
Solid State ◽  
Hydrogen Bonds ◽  
Single Crystal ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
State Structure ◽  
X Ray Diffraction ◽  
Space Group ◽  
Solid State Structure ◽  
X Ray

The solid-state structure of N,N-dibenzylhydroxylamine (1) has been determined by single crystal X-ray diffraction. The compound crystallizes in the monoclinic space group P 21/n with four formula units in the unit cell. N,N-dibenzylhydroxylamine dimerizes to give N2O2H2 sixmembered rings as a result of the formation of two hydrogen bonds O - H ··· N in the solid state.

Solid-state and solution 117Sn NMR study of C2O4(SnPh3)2: a revision

2011 ◽  
Vol 34 (5-6) ◽  
pp. 153-153
Author(s):  
Libasse Diop
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Solid State ◽  
Magnetic Resonance ◽  
State Structure ◽  
X Ray Diffraction ◽  
Magnetic Resonance Studies ◽  
X Ray ◽  
Nmr Study ◽  
Tetrahedral Environment ◽  
Good Agreement

Abstract Solid-state and solution 117Sn nuclear magnetic resonance studies of C2O4(SnPh3)2 have been carried out and found to be in good agreement with the tetrahedral environment of the tin (IV) atom as found from the solid state structure, previously determined by a single crystal X-ray diffraction analysis.

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