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41.
Verma SK Nguyen QH MacDougall JM Fleischer EB Moore HW 《The Journal of organic chemistry》2000,65(11):3379-3386
6-exo-Methylbicyclo[3.2.0]hepten-7-ones and their 2-alkylidene analogues are readily prepared from dialkyl squarates. These compounds undergo facial oxy-Cope ring expansions upon treatment with vinyllithium; the former leads to bicyclo[4.2. 1]non-1(4)-en-6-ones and the latter to the first examples of bicyclo[5.2.1]dec-1(10)-en-5-ones, compounds having exceptionally strained bridgehead double bonds. The transformations are controlled by the 6-exo-methyl group in the starting material along with the substituent at position-1 (bridgehead) which force attack of the lithium reagent from the concave face of the starting material, thus allowing the cyclopentenyl or alkylidene groups to participate in the sigmatropic event. 相似文献
42.
A method is proposed for the determination of bromine in organic compounds (which may also contain chlorine and iodine) by oxygen-flask combustion of the compound followed by pre-column reaction of bromide with acetanilide and 2-iodosobenzoic acid to form 4-bromoacetanilide which is then chromatographed on an ODS column with a mobile phase of methanol: water, 65:35 v/v, detection at 240 nm, and 4-N-acetylaminotoluene as internal standard. The method is rapid and precise (RSD = 1%), and applicable to a variety of bromine-containing organic compounds; the limit of detection is 0.2 ng of bromine. 相似文献
43.
Thiourea and its organic derivatives and thiosemicarbazide are determined in water, methanol or glacial acetic acid medium by reaction with an excess of iodine trichloride in the presence of mercuric chloride. The reaction is complete in 15 min. The excess of iodine trichloride is evaluated by adding potassium iodide and titrating the liberated iodine with thiosulphate. A variety of organic thioureas can be determined with an average accuracy and precision of 0.2%. 相似文献
44.
(C6H5)3MX2 (M = As, Sb; X = OCOCF3 and M = Sb, Bi; X = SO3F, SO3CF3) compounds prepared by the interaction of triphenylmetal(V) substrates with (CF3CO)2O, (CF3SO2)2O and (FSO2)2O have been characterized by molecular weight determination, elemental and spectroscopic (IR, 1H and 19F NMR, mass) analyses. 相似文献
45.
Background correction has been shown to be an effective and indispensable modification in the spectrophotometric determination of ascorbic acid. The decomposition of ascorbic acid in pharmaceutical samples was carried out by incubation with sodium hydroxide to give products that were insensitive to ultraviolet light. The rapid oxidation in air of ascorbic acid, especially in dilute solutions, was avoided by the use of the flow injection principle for spectrophotometric determination and by employing a carrier stream of an anti-oxidizing nature consisting of 6 micrograms ml(-1) of 2-mercaptoethanol in 0.25% sulphuric acid. The optimized method with a single channel manifold made use of a carrier stream flow rate of 1.1 ml min(-1), an injection volume of 50 microl, a delay coil of 50 cm (0.5 mm i.d.) and detection at 245 nm. The throughput was at least 180 injections h(-1). The proposed flow injection method yielded results for the analysis of 0-20 micrograms ml(-1) of ascorbic acid that were 99-102% (relative standard deviation 0.6% or better) in agreement with those produced by comparable methods involving titration with iodine, chloranil or 2,6-dichlorophenolindophenol [4-(2,6-dichloro-4-hydroxyphenylimino)cyclohexa-2,5-dieno ne], and high-performance liquid chromatography. When the agreement was not good (as low as 14% with respect to the method being compared), this was traced to the presence of substances which are known to interfere in one or other of the methods of comparison. 相似文献
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BaSeO3·2·5H2O(I), PbSeO3· 2H2O(II) and CdSeO3·3.5H2O(III) were prepared and analysed. Their hygroscopicity and solubility was investigated. These compounds have high thermal Stability, as shown by their TG and DTA data. IR spectra show multi-dentate coordination of selenite to cations, due to considerable splitting of the asymmetric v3 and v4 bands of SeO
3
2
– in the 780-730 cm–1 and 420-325 cm–1 region.Tentative structures have been proposed involving bridging oxygen atoms.
Zusammenfassung BaSeO3-2.5H2O(I), PbSeO3 · 2H2O(II) und CdSeO3· 3.5H2O(III) wurden hergestellt, analysiert sowie deren Hygroskopizität und Löslichkeit untersucht. TG- und DTA-Untersuchungen erweisen die hohe thermische Stabilität dieser Verbindungen. Die IR-Spektren zeigen mehrzählige Koordination von Selenit zu Kationen, was aus einer beträchtlichen Aufspaltung der antisymmetrischenv 3 undv 4 Banden von SeO 3 2 – im Bereich 780-730cm–1 bzw. 420-325 cm–1 hervorgeht. Es wurden versuchsweise Strukturen mit überbrückenden Sauerstoffatomen vorgeschlagen.
BaSeO3· 2,5H2O, PbSeO3 · 2H2O CdSeO3 · 3,5H2O . . - , v 3 v 4 SeO 3 2 }- 780-730 420-325 –1. , .相似文献
50.
Procedures are described for the determination of organic compounds with iodine trichloride under Andrews's titration conditions. Samples are directly titrated with iodine trichloride or first reacted with an excess of iodine monochloride, with subsequent titration of the iodine formed. The direct titration is done initially in feebly acid medium, then the acidity is raised (biotin, methionine, cystine and thiomersal). Pre-oxidation with iodine monochloride is used if the organic compound reacts slowly [tryptophan and arsenic(III) compounds] or is determined in bicarbonate medium (hydroxylamine and thiosemicarbazide). The ferrocyanide formed by the reduction of ferricyanide (by thiourea and allylthiourea) can also be titrated. Arsenic(V) compounds are determined after reduction to arsenic(III), and iodine in organic compounds is converted into iodide by alkaline fusion into iodide and the iodide titrated. 相似文献