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971.
Conjugated esters and amides react with aryldiazonium salts at room temperature (MeCN) to form the corresponding iminium hydrazone derivatives, which can be thermally cyclized to cinnoline-3-esters and cinnoline-3-amides. In general the intermediate iminium salts derived from the enamine amides cyclize faster than those from the enamine esters. Furthermore, the ease of cyclization depends upon the structure of the base-component of the enamine ester or the amide and the substituent in the aryl moiety of the diazonium salt. The configurational structure of the iminium hydrazones, studied by NMR spectroscopy, has been shown to involve H-bonding of the hydrazonyl N-H with the ester or the amide CO group. 相似文献
972.
Günter Haufe Manfred Mühlstädt Dr. Jürgen Graefe 《Monatshefte für Chemie / Chemical Monthly》1977,108(4):803-811
In addition totrans-2-bromocyclooctanol andtrans-1,2-dibromocyclooctane,cis-4-bromocyclooctanol,cis-1,4-dibromocyclooctane,trans-1,4-dibromocyclooctane, and (Z)-5-bromocyclooctene are obtained, when (Z)-cyclooctene is treated with N-bromosuccinimide in the presence of water. Similarly the methoxybromination of (Z)-cyclooctene gives transanular products. 相似文献
973.
The rapid gas chromatographic detection and determination of ethylene glycol in biological fluids is described. Phenylboronic acid in acetone was used for the esterification of glycol. The phenylboronates of ethylene glycol and 1,2-propylene glycol are not separated on a packed column of medium polarity (OV-17), but they can be separated on a non-polar column (OV-101). In both instances, 1,3-propylene glycol can be used as an internal standard. The method requires only 100 microliters of serum or urine and is suitable for trace analysis in an emergency toxicological laboratory. The utility of the method is demonstrated on two cases of human intoxication with ethylene glycol. 相似文献
974.
The efficient degradation of to the α-methylene ketone is described. Compound was then converted to the allylic alcohol - the precursor of vitamin D3 relatives. 相似文献
975.
Studies on Alkyl Metal Alkoxides of Aluminium, Gallium, and Indium. III. Properties and Vibrational Spectra of Dialkylgallium- and Indium Alkoxides The preparation and the properties of dialkyl metal alkoxides R2MOR′ (with R = CH3, CD3, C2H5; R′ = CH3, CD3 and M = Ga, In) are described. The vibrational data (IR and Raman) of the trimeric methyl derivatives point to puckered six-membered M3O3-ring systems. 相似文献
976.
Quinolizidines containing an exocyclic double bond at C-2 (1,2) give on mild oxidation the amino dienes (3,4), as mixtures of geometric isomers with respect to the exocyclic double bond. The free enthalpy of activation for the rotation about the double bond has been estimated by NMR. 相似文献
977.
Chalcogenolates and their Derivatives. I. Syntheses and Properties of Ionic Chalcogenophenolates The syntheses and properties of ionic chalcogenophenolates are described. Using liquid ammonia as solvent the alkali chalcogenophenolates M[EPh] (M = Na, K; E = Se, Te; Ph = C6H5) have been synthesized via reduction of the diphenyl dichalcogenides with alkali metals. Similarly, the tetraphenylphosphonium chalcogenophenolates [Ph4P][EPh] (E = S, Se, Te) have been obtained by reacting alkali chalcogenophenolates with tetraphenylphosphonium chloride. 相似文献
978.
The influence of the buffering medium on the reaction of Hg(II) with Xylenol Orange has been studied. Amine-type compounds are complexed by Hg(II)/Xylenol Orange with a sharp hyperchromic effect on the reagent itself, at 590 nm, but complex formation of Hg(II)/Xylenol Orange in non-amine-type buffer, such as citric acid-phosphate, gives a hypochromic effect on Xylenol Orange at 580 nm. Hg(II) is determined at pH 7.5 in two ranges of concentration, 2-9 ppm in citrate buffer, measured at 580 nm ( = 2.50 x 10(4)), and 6-11 ppm in hexamine buffer, at 590 nm ( = 4.18 x 10(4)). 相似文献
979.
The behaviour of the oxinates of niobium, tantalum and associated metals in the infra-red region was studied and a method developed for the determination of niobium and tantalum. Vanadium caused no interference, but other heavy metals, such as molybdenum, manganese and cobalt, which interfered were removed by preliminary treatment when the method was applied to the determination of niobium and tantalum in steels. 相似文献
980.
Abstract— –By e.s.r. we have studied the photoexcitation of an aromatic amine to its triplet state at 77°K, its photoionization to a radical cation and the simultaneous formation of solvent radicals proceeding from the photosensitization of the organic glassy matrix. In the case of methanol and ethanol matrix we observe approximately one solvent radical per solute radical cation. In the case of isopropanol and methyltetrahydrofuran we find respectively three and two solvent radicals per solute radical cation. The results suggest two possible processes of photosensitization. By successive absorption of two photons, the amine reaches an excited triplet state which is able either to dissociate giving one electron and one cation radical or to transfer its energy to the solvent, this last being decomposed. It is assumed that in the case of methanol and ethanol, the radicals from the solvent are only formed by reaction on the matrix by the released electron, whereas in the case of isopropanol and methyltetrahydrofuran, the second process is prevalent or exclusive. 相似文献