Condensation du complexe hexafluoroacetone - fluorure de potassium sur les cetones alpha - halogenees

During its condensation with α-halo ketones, the hexafluoro- acetone-potassium fluoride complex behaves as a weak nucleophile and a strong base. Nucleophilic substitution produces α-perfluoroalkoxy ketones. Abstraction of a proton α to the carbonyl function leads to the formation of ether-ketones substituted by the group C(CF₃)₂. In some cases, hydrogen halide elimination can occur.     

Stereospecific total synthesis of (±)-strempeliopine

The 18-methylene-1,2-dehydroaspidospermidine (III) was stereospecifically transformed into the schizozygane alkaloid strempeliopine (II) in 16,6 % overall yield.     

Structure and PMR spectra of isoquercitrin and hirsutrin

Chemistry of Natural Compounds - 1. Two isomers of quercetin 3-glucoside are present in the flowers and leaves of the cotton plant of variety 108-F: hirsutrin, quercetin 3-β-D-glucopyranoside;...     

Simultaneous determination of butyltin and phenyltin species in sediments using ultrasound-assisted leaching

A fast and simple procedure is presented for the simultaneous leaching of butyl (mono, di and tributyl) and phenyl organotin species from sediment samples. Leached compounds are further ethylated with sodium tetraethylborate in aqueous medium, and analyzed by gas chromatography. After testing the stability of triphenyltin under different extraction conditions, ultrasound-assisted leaching at room temperature in the presence of acetic acid was been proposed as an extraction procedure compatible with the simultaneous determination of phenyl- and butyltin compounds in sediments. Recoveries between 70 and 90% were obtained for phenyl species in spiked samples prepared in the laboratory. Results for butyltin species were validated by use of the reference material PACS-2. Quantification limits, using GC-MIP-AES as measurement technique, were approximately 5-10 ng g(-1). Precision in the consecutive analysis of three sediment samples varied between 3 and 10%.     

Separation and determination of podophyllum lignans by micellar electrokinetic chromatography

A micellar electrokinetic chromatography method was established for the quantitative analysis of seven podophyllum lignans in Podophyllum emodi Wall. var. chinesis sprague. The optimum buffer system was 10 mM NaH2PO4-5 mM borate-100 mM sodium dodecylsulfate-30% isopropanol (pH 7.20). Voltage was 18 kV and detection at 214 nm. The second derivative chromatogram was used to determine a low-content component and those not fully separated from adjacent ones. The RSD values of migration times and peak areas were <2.2 and <5.5%, respectively. The effects of several CE parameters on the resolutions were studied systematically.     

Oxidative dehydrogenation of C5 hydrocarbons in the presence of hydrochloric acid

Conclusions The oxidative dehydrogenation of C₅ paraffin hydrocarbons on Fe catalysts in the presence of HCl leads mainly to the formation of unsaturated hydrocarbons, which have the same structure of the carbon skeleton as the starting hydrocarbon, in which connection the yield of olefinic hydrocarbons proved to be substantially higher (25% from isopentane and 32% from n-pentane) than the yield of dienes (respectively 15% of isoprene and 11% of piperylene).Translated from Izvestiya Akademii Nauk SSSR, Seriya Khimicheskaya, No. 11, pp. 2599–2601, November, 1972.     

Analysis of hydroquinone and some of its ethers by using capillary electrochromatography

Capillary electrochromatography (CEC) was used for the analysis of relevant compounds in cosmetic preparation. Hydroquinone (HQ) and some of its ethers (methyl-, dimethyl-, benzyl-, phenyl-, propyl-HQ derivatives) were analyzed by using an octadecylsilica (ODS) stationary phase packed in fused-silica capillary (100 microm I.D.; 30 cm and 21.5 cm total and effective lengths, respectively). 20 mM Ammonium acetate pH 6-acetonitrile (50-70%) were the mobile phases used for the experiments. The acetonitrile (ACN) content strongly influenced the resolution of the studied compounds as well as the efficiency and the retention factor. Baseline resolution for the studied analytes was achieved at both the lowest and the highest percentage of ACN, the last one providing the shortest analysis time. Mobile phase containing 70% of ACN was therefore used for the analysis of an extract of skin-toning cream declared to contain HQ. Good repeatability of both retention times, peak areas and peak areas ratio (Asample/Ainternational standard) was found. The calibration graphs were linear in the concentration range studied (5-90 microg/ml) with correlation coefficients between 0.9975 and 09991. The analysis of the cosmetic preparation revealed the presence of HQ (1.72%, w/w) and of two additional peaks (not identified).