Negative ion FAB mass spectroscopy of some ribose alkylated 5'-UMP derivatives

Characteristic fragment ions obtained in Fast atom bombardment (FAB) mass spectroscopy of ribose alkylated Uridine 5'-monophosphate (5'-UMP) derivatives in negative ion mode are described. All the compounds examined exhibited either [M]- or quasimolecular ion [M - H]- the fragmentations can be used to characterize these nucleotides.     

Transmission electron microscopy and X-Ray diffraction analysis of aluminum-induced crystallization of amorphous silicon in alpha-Si:H/Al and Al/alpha-Si:H structures.

Solid phase crystallization of plasma-enhanced chemical-vapor-deposited (PECVD) amorphous silicon (alpha-Si:H) in alpha-Si:H/Al and Al/alpha-Si:H structures has been investigated using transmission electron microscopy (TEM) and X-ray diffraction (XRD). Radiative heating has been used to anneal films deposited on carbon-coated nickel (Ni) grids at temperatures between 200 and 400 degrees C for TEM studies. alpha-Si:H films were deposited on c-Si substrates using high vacuum (HV) PECVD for the XRD studies. TEM studies show that crystallization of alpha-Si:H occurs at 200 degrees C when Al film is deposited on top of the alpha-Si:H film. Similar behavior was observed in the XRD studies. In the case of alpha-Si:H deposited on top of Al films, the crystallization could not be observed at 400 degrees C by TEM and even up to 500 degrees C as seen by XRD.     

SOME HETEROCYCLIC PHOSPHOROCHLORIDATES AND THE FORMATION OF OTHER HETEROCYCLIC ORGANOPHOSPHORUS COMPOUNDS

Abstract

Pyrrolidine, morpholine, and β-hydroxyethylmorpholine have been phosphorylated with phosphorus oxychloride, phenylphosphorodichloridate, p-chlorophenylphosphorodichloridate and thiophosphoryl chloride. The resultant phosphorodichloridates have been condensed with a wied range of nucleophilic reagents, e.g. amines, hydrazines, phenols and isobutanol. Piperazine with phosphorus oxychloride (2 mols) gave the N(1) N(4)-diphosphorotetrachloridate, which was characterized as the tetracyclohexylamidate. β-Hydroxyethylpiperazine was similarly phosphorylated to the N,O-diphosphorotetrachloridate which was characterized as the tetraphenylhydrazidate.

Condensation of pyrrolidine (2 mols) with phosphorus oxychloride (1 mol) afforded N,N′-dipyrrolidinophosphorochloridate which was reacted with phenylhydrazide and sodium azide. The phosphoroazide with triphenylphosphine afforded the corresponding triphenylphosphinimine. N-Phenyl N′-pyrrolidinophosphorochloridate with aqueous pyridine gave the corresponding pyrophosphoramide and the stability of the pyrophosphoramide towards hydrolysis was examined. 1,2-Cyclohexanediol was phosphorylated with phenylphosphorodichloridate and thiophosphorylchloride. Trans-4-t-Butylcyclohexyl N,N′-diphenylhydrazinophosphorothioate by reaction with formaldehyde gave a tetra-azaphosphorine P-sulfide. Trans-4-t-Butylcyclohexyl N-phenyl N′-phenylphosphorodiamidic hydrazide reacted with 1,4-dibromobut-2-ene to give a 1,2-diazahex-4-ene.     

A Convenient Synthesis of β-Amino Acid

We have reported the reductive cleavage of azlactones¹ and phenylhydrazones² of carbonyl compounds in the presence of a suitable catalyst. In this paper a general method involving a one step synthesis of β-amino acid^3,4, in good yield, through catalytic reduction of oximes of α-β-unsaturated acid is reported. This method involves the reaction of α, β-unsaturated acid with hydroxylamine hydrochloride in the presence of sodium acetate. Markovnikov's rule is followed in the synthesis of oximes of α, β-unsaturated acids.     

Highly efficient deprotection of phenolic tetrahydropyranyl and methoxymethyl ethers and sequel cyclization to indanones using Sn(IV)Cl4 catalyst

Sn(IV)Cl₄ catalyst provided a rapid and efficient deprotection method for the phenolic THP and MOM ethers and sequel intramolecular Friedel–Crafts alkylation reaction of THP and MOM protected chalcone epoxides under mild conditions. The reaction took 2–3 min to give the products in excellent yield (90–98%) at 0 °C without affecting the other functional groups.     

Formation of a Single-Crystal Aluminum-Based MOF Nanowire with Graphene Oxide Nanoscrolls as Structure-Directing Agents

An innovative strategy is proposed to synthesize single-crystal nanowires (NWs) of the Al³⁺ dicarboxylate MIL-69(Al) MOF by using graphene oxide nanoscrolls as structure-directing agents. MIL-69(Al) NWs with an average diameter of 70±20 nm and lengths up to 2 μm were found to preferentially grow along the [001] crystallographic direction. Advanced characterization methods (electron diffraction, TEM, STEM-HAADF, SEM, XPS) and molecular modeling revealed the mechanism of formation of MIL-69(Al) NWs involving size-confinement and templating effects. The formation of MIL-69(Al) seeds and the self-scroll of GO sheets followed by the anisotropic growth of MIL-69(Al) crystals are mediated by specific GO sheets/MOF interactions. This study delivers an unprecedented approach to control the design of 1D MOF nanostructures and superstructures.     

Determination of zinc(II) in biological samples by anodic stripping voltammetry

The use ofN-benzyltrimethylammonium methoxide as a digesting solvent, for the determination of zinc(II) in biological samples using anodic-stripping voltammetry is reported. It was found possible to determine zinc directly in biological samples containing such metals as copper(II), lead(II), iron(III), arsenic(III) and selenium(IV). The results for zinc in bovine liver and oyster tissue are reported.     

Structure determination of salisomide and salisoflavan,two new secondary metabolites from Salsola imbricata,by 1D and 2D NMR spectroscopy

Chromatographic analysis of the alcoholic extract from Salsola imbricata yielded two new secondary metabolites, salisomide (1) and salisoflavan (2). Their structures were established with the help of spectroscopic techniques including COSY, HMQC and HMBC NMR experiments. Copyright © 2008 John Wiley & Sons, Ltd.     

Encapsulation and characterization of flurbiprofen loaded poly(є-caprolactone)–poly(vinylpyrrolidone) blend micropheres by solvent evaporation method

Flurbiprofen loaded PCL/PVP blend microspheres were prepared by o/w solvent evaporation method using various concentrations of gelatin as emulsifying agent. Microsphere recovery decreased with a decrease in the concentration of the emulsifier in the dispersion. Encapsulation efficiency and drug loading of microspheres increased with decrease in concentration of emulsifying agent. Hydration rate, encapsulation efficiency and drug loading of microspheres increased with increase in concentration of PVP. Rheological properties showed free flowing nature of microspheres. SEM (Scanning electron microscope) revealed microspheres were discrete, spherical and became porous with decrease in concentration of emulsifying agent but smooth with higher concentration of emulsifying agent. FTIR (Fourier transform infrared spectroscopy) spectra of pure and encapsulated flurbiprofen in all formulation showed no significant difference in characteristic peaks, suggesting stability of flurbiprofen during encapsulation process. X-RD (X-ray powder diffractometry) of pure flurbiprofen shows sharp peaks, which decreases on encapsulation, indicating dispersion at molecular level and hence decrease in the crystallinity of drug in microspheres. Microspheres showed an enteric nature at pH 1.2 and a sustained release pattern at pH 6.8. Rapid drug release was observed in microspheres with higher concentration of PVP (polyvinylpyrrolidone), PVP acts as channeling agent. Formulation with low concentration of emulsifying agent also showed a fast release due to porous structure. Drug release kinetics followed zero order at pH 1.2 while at pH 6.8 Higuchi model was best fitted and was found non fickian.