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1.
A simple, efficient and highly chemoselective method for tetrahydropyranylation of alcohols and phenols has been developed by their reaction with 3,4-dihydro-2H-pyran at room temperature in the presence of a catalytic amount of polystyrene supported AlCl3. The method is also highly selective for monoprotection of symmetrical diols. 相似文献
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Deuterium labeling in the acetate derivatives of cholic acid demonstrates that electron impact induced consecutive loss of HOAc from the molecular ion occurs in the following order of decreasing preference: 12α-OAc > 7α-OAc > 3α-OAc. Numerous examples are presented showing that consecutive loss of HOAc from a common ion generally increases progressively with relative intensity. In the acetate pregnan-20-one derivatives of cholic acid, loss of 43 mass units from the molecular ion comes from the 12α-OAc and not the 17β-acetyl sidechain. Ketene is ejected from an acetoxy group located in an α position to a carbonyl on which an ion-radical charge is localized. 相似文献
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In this work, a simple and rapid analytical procedure was applied for simultaneous determination of folic acid (vitamin B0), thiamin (vitamin B1), riboflavin (vitamin B2) and pyridoxal (vitamin B6) based on the absorbance data in the pH range 2.0‐12.0 at 25 °C using parallel factor analysis (PARAFAC). The effect of the pH as the most important factor on the sensitivity of the determination was studied. The spectral data were recorded in 400‐650 nm intervals and a 2‐12 pH range for all four vitamins. The calibration set was constructed in the concentration ranges of 4‐22, 1‐20, 6‐26, and 4‐20 μg mL?;1 for B6,B2,B1 and B0, respectively. The root mean squares errors of prediction for the prediction set, (RMSEP), are 0.65, 0.63, 1.13 and 0.34 for B0,B1,B2 and B6, respectively. The recovery percent for the validation set are in the range of 90.6 to 107.0%. The effect of the experimental conditions and diverse species were discussed. The optimum values of these factors were searched according to the relative standard deviation of the prediction set of mixtures solutions. 相似文献
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Possibility of imide structure formation under microwave irradiation of molecules containing anhydride and isocyanate functional groups was investigated. The microwave-assisted polycondensation of aromatic diisocyanates and dianhydrides for preparation of polyimides was studied. The effect of microwave irradiation time and power, solvent nature, solid content of monomers, effect of catalyst, effect of polymerization reactor material and possibility of pressure development during polymerization, on the inherent viscosity of prepared polyimides were discussed. Experimental results showed that polymers obtained via this method had superior inherent viscosity and yield in comparison to the polymers obtained via conventional solution method. 相似文献
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Analogy and deuterium labeling demonstrate that considerable remote group interaction occurs between functional groups at positions 7 and 16 in 16, 17-secosteroids. It is proposed that ion-dipole interact?ions separations of distances of 10 to 2 Å will involve energies of 1–30 kcal mol?1 and can play a significant role in fragmentation processes. Successive loss of one, two and three HOAc molecules from a milecular or daughter ion increase progressively in relative intensity; irregularity in this pattern indicates the operation of special factors or multiple genesis of daughter ions having the same m/e. Evidence is presented which suggests that facile ketene ejection from the acetate functional group only occurs from a radical ion and must be preceded by transfer of a hydrogen radical from the acetate group to the site of charge localization. 相似文献
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On-line preconcentration system for the selective, sensitive and simultaneous determination of chromium species was investigated. Dual mini-columns containing chelating resin were utilized for the speciation and preconcentration of Cr(III) and Cr(VI) in water samples. In this system, Cr(III) was collected on first column packed with iminodiacetate resin. Cr(VI) in the effluent from the first column was reduced to Cr(III), which was collected on the second column packed with iminodiacetate resin. Hydroxyammonium chloride was examined as a potential reducing agent for Cr(VI) to Cr(III).The effects of pH, sample flow rate, column length, and interfering ions on the recoveries of Cr(III) were carefully studied. Five millilitres of a sample solution was introduced into the system. The collected species were then sequentially washed by 1 M ammonium acetate, eluted by 2 M nitric acid and measured by ICP-AES. The detection limit for Cr(III) and Cr(VI) was 0.08 and 0.15 μg l−1, respectively. The total analysis time was about 9.4 min.The developed method was successfully applied to the speciation of chromium in river, tap water and wastewater samples with satisfied results. 相似文献
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Bahman Parsa 《Journal of Radioanalytical and Nuclear Chemistry》1992,157(1):65-73
A sequential radiochemical procedure for isotopic analysis of uranium and thorium in soil has been developed. Analysis involves total dissolution of the samples to allow equilibration of the natural isotopes with added tracers, followed by radiochemical separation using anion exchange chromatography (BioRad AG 1–X8). Further separation and purification is performed employing solvent extraction techniques. Finally, the U and Th fractions are co-precipitated with lanthanum and cerium fluoride, respectively, and quantified by alpha-particle spectrometry. Overall chemical yields range from 60 to 90%. Under normal operating conditions and present counting set up, the minimum detectable concentration (MDC) is approximately 2 Bq/kg for soil samples. This is based on one gram aliquot of sample, 80% chemical yield, and 1000 minute counting with a detector having about 15% counting efficiency. The procedure has been successfully tested with Standard Reference Materials. Various soil samples were analyzed with high chemical yields and fine quality of alpha-spectra. Decontamination factor studies were performed to determine the extent of the carry over of210Po,225Ac,226Ra, and229Th into U fraction and210Po,225Ac,226Ra, and232U into Th fraction. 相似文献