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61.
The fragmentation patterns of 3-methyl-2-butyl trifluoroacetate and 2-methyl-2-butyl trifluoroacetate were investigated by GC/MS/MS, with electron impact and collision-induced dissociation, on regular and isotope-labeled (deuterium and 18O) esters. The atoms found in various fragments could be traced back to specific positions in the parent molecules. In this way, molecular rearrangements potentially occurring during the formation of esters by trifluoroacetolysis of 3-methyl-2-butyl p-toluenesulfonate or trifluoroacetic acid addition to various 2-methylbutenes could be shown. Rearrangements also occurred during the fragmentation, particularly during the expulsion of the small fragments CO, C2H4 and F2CO. For the decompositions of oxygen-containing ions these rearrangements were highly specific. By contrast, alkyl cations lead to fragments that are fully scrambled (statistical label distribution). Alkene radical cations ([CnH2n]+ ˙) fragment to daughter ions that are extensively, but less than statistically scrambled. Hydrogen scrambling may also occur in fluoroalkyl cation fragments. 相似文献
62.
Tiao-Hsu Chang 《中国化学会会志》1966,13(4):143-149
The acid dissociation constants of dihalogenated 8-hydroxyquinaldines and the stability constants of their chelates with Zn[II], Ni[II], Co[II], Pb[II], Cd[II], Mn[II], and Mg[II] have been determined. The Calvin-Bjerrum potentiometric titration technique was used in studying the behavior of these substances. The order of decreasing stability of the metal chelates Zn, Nc>Co>Pb>Cd>Mn>Mg is similar to the stability sequence generally obtained for divalent metals, and the order of decreasing stability of dihalogenated 8-hydroxyquinaldines to form the metal chelates with metal ions is I>Br>Cl. Spot test reactions of dihalogenated 8-hydroxyquinaldines and 8-hydroxyquinolines with the metal ions also have been investigated. 相似文献
63.
The mixture of silver iodide and ferrocene is used to prepare the membrane of iodide ion-selective electrode. The interference of sulfide can be reduced by the addition of cupric ion in the test solution. Ethylene glycol is determined by potentiometric titration using iodine ion-selective electrode as an indicator electrode. 相似文献
64.
Very low pressure photolysis (VLPØ) of chlorine nitrate was performed in a quartz Knudsen cell. The light source was a 2500 W high-pressure xenon lamp, and a modulated molecular-beam mass spectrometer was used to monitor the concentration of ClONO2 and photolysis products. Because of the low pressures used (? 10?3 torr) and the short residence time in the cell (≈1 s), secondary reactions were unimportant and the primary products could be directly identified. The primary photolysis products (λ ≈ 2700 Å) are atomic chlorine and NO3 free radical. Chlorine atoms were identified both by the appearance of Cl2 (wall recombination product; the walls were not poisoned) and by HCl produced when C2H6 was added to the cell. Nitrate free radical was directly identified as a mass peak at m/e = 62, as well as by chemical titration with nitric oxide: NO3 + NO → 2NO2. It was verified by direct tests that the peak at m/e = 62 did not arise from possible HNO3 contamination or from N2O5, a possible secondary product. This titration reaction was used to measure quantitatively a lower limit to the primary quantum yield, φ ? 0.5 ± 0.3. This represents a lower limit because of the unknown extent of the secondary photolysis of NO3 under our conditions. We believe this to be the first observation using mass spectrometry of the NO3 free radical. The quantum yield for atomic chlorine is φ = 1.0 ± 0.2. N2O was used to test for O(1D) according to the reaction, O(1D) + N2O → products; none was observed. Triplet oxygen, O(3P) was observed to the extent of ≈ 10% by the reaction O(3P) + NO2 → NO + O2, but this yield can also be due to the photolysis of NO3 free radical produced in the primary step. We conclude that the predominant reaction pathway is . 相似文献
65.
A homogeneous catalyst, 3-benzyl-5-(2-hydroxyethyl)-4-methyl-1,3-thiazolium chloride, for addition of aldehydes to activated double bond, was attached to 20% cross-linked polystyrene-divinylbenzene copolymer. The attached catalysts could be easily removed from the reaction mixture. Polymer-attached thiazolium salts in the presence of triethylamine are active catalysts for addition of aromatic and aliphatic aldehydes to α,β-unsaturated ketones to yield γ-diketones. 相似文献
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