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51.
Treatment of 3,4-alkadienyl carbonates 2a-i with a low-valent titanium reagent diisopropoxy(eta(2)-propene)titanium (1), readily generated by the reaction of Ti(O-i-Pr)(4) with 2 i-PrMgCl, resulted in an intramolecular nucleophilic acyl substitution (INAS) reaction to afford vinyltitanium compounds 3 which, in turn, reacted with H(3)O(+), D(2)O, or iodine to give alpha-substituted beta,gamma-unsaturated esters 4 in good to excellent yields. The olefin moiety of the hydrolysis product 4 has (Z)-geometry mainly except for 4h. Starting from chiral 2f or 2g, the reaction proceeded stereospecifically to give optically active alpha-substituted beta,gamma-unsaturated ester 4f or 4g having (Z)-olefin geometry exclusively. 相似文献
52.
Fernandes SA Nachtigall FF Lazzarotto M Fujiwara FY Marsaioli AJ 《Magnetic resonance in chemistry : MRC》2005,43(5):398-404
'Non-covalent synthesis' of novel chiral hosts (calix[6]arene-chiral amine complexes) and its application to enantiomeric discrimination was investigated by (1)H NMR spectroscopy. The topology of a ternary complex was proposed for the calix[6]arene-amine-sulfoxide to rationalize the chiral recognition. 相似文献
53.
Base-catalyzed reaction of 5-acylmethyl-2,5-di--butyl-4-oxa-2-cyclopentenones selectively derived from 4-alkyl-2,6-di--butylphenols three steps involving oxygenation, acetylation, and acid-treatment gave 3-alkyl-2,5-di--butyl-2,4-cyclopentadienones in excellent yield. 相似文献
54.
Anionic surfactants are preconcentrated from 5-ml samples by extraction as the ion-pair with ethyl violet into toluene. The absorbance of aliquots of the toluene phase is measured at 610 nm in a flow-injection system. A phase converter is located prior to the injection valve to convert a water stream to, pumped with ordinary pump tubing, to a toluene stream. The working range was 0.01–1.0 mg l?1 and the reproductibility (r.s.d, n = 10) was 2% for 0.4 mg l?1 sodium dodecyl sulphate. The non-aqueous flow-injection system serves to miniaturize the extraction from separatory funnel (200 ml) to test tube (10 ml) scale without loss of precision or validity. 相似文献
55.
G. Tamai H. Yoshida H. Imai T. Takashina K. Kotoo T. Fuwa Y. Tsuchioka H. Matsuura G. Kajiyama 《Chromatographia》1985,20(11):671-676
Summary New quinidine metabolites, including 10,11-dihydrodiol quinidine N-oxide, 10,11-dihydrodiol quinidine and their glucuronides, were found in human urine. A quinidine monitoring HPLC method including these metabolites, is proposed by the direct injection of body fluid samples onto the precolumn for deproteinization followed by reverse phase separation in the analytical column with a column switching technique. The recovery of spiked quinidine and its metabolites in plasma was quantitative (98–102%) with good reproducibility (C.V.: 1.6–4.0%). Several clinical samples such as whole blood and urine were analyzed by the present method. 相似文献
56.
Reaction of 5-formyl-1,3-dimethyluracil with some active methylene compounds in the presence of base causes novel ring transformations to give the p-hydroxybenzoates and the nicotinate. 相似文献
57.
58.
A rate equation for photodegradation was derived from Lambert-Beer's law and Grotthus-Draper's law: -dc/dt=k1(1-exp(-(k2c+k3(c0-c))))k2c/(k2c+k3(c0-c)) where c is the concentration of reactant, c0 is the initial concentration of reactant, t is time, k1 is the rate constant, and k2 and k3 are the absorption coefficient of reactant and its photodegradation product, respectively. In a case where the photodegradation products have no photoabsorption, k3 assumes the value of zero in the above general equation. In a case where the photodegradation products have the same spectrum and molar absorptivity as that of the reactant, k3 assumes the value of k2, and hence the photodegradation is not a first-order reaction; however, the equation itself gives the pseudo-first-order reaction rate equation. In a case where the concentration of reactant is high enough, the equation approaches a zero-order reaction rate equation. The photodegradation rate of nifedipine in solutions under a germicidal lamp, near an ultraviolet fluorescent lamp and a fluorescent lamp was analyzed using the above equation. The photodegradation rate was directly proportional to the amount of light absorbed, and fitted well with the equation. The above theoretical equation was substantiated by the photodegradation of nifedipine, and hence is expected to apply to other photosensitive drugs. 相似文献
59.
60.
Ji-Ben Meng Mei-Qen Shen Xiao-Hong Wang Chen-Heng Kao Ru-Ji Wang Hong-Gen Wang Teruo Matsuura 《Journal of heterocyclic chemistry》1991,28(6):1481-1484
A number of fluorescent 3-aryl-1-methylquinolinones 3 were synthesized by the regiospecific photocoupling reaction of 3-halo-1-methylquinolinones 1 with aromatic and heteroaromatic compounds 2 . An unusual photocoupling product 4 was obtained in the photolysis of 3-iodo-1-methylquinolinone in the presence of benzene. The structure of 4 was unequivocally established by an X-ray crystallographic analysis. 相似文献