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31.
Kenneth Turnbull Thomas L. Blackburn Daniel T. Esterline 《Journal of heterocyclic chemistry》1990,27(5):1259-1263
Bromination of the sydnone ring of several ortho-substituted N-arylsydnones is reported. Subsequent side-chain modification generally can be achieved without concomitant removal of the 4-bromo protective group. 相似文献
32.
Kenneth L. Rinehart 《Trends in analytical chemistry : TRAC》1983,2(1):10-14
Fast atom bombardment mass spectrometry (FABMS) is a powerful new structural tool. Ionization is effected by bombarding a glycerol matrix with neon or argon atoms of 5–10 KeV energy. Positive and negative secondary ions are sputtered from the surface and can be detected for inorganic ion clusters to mass 25 800 and biologically important compounds to mass 5 700. FABMS is especially valuable in determining the sequence of amino acids in polypeptides. 相似文献
33.
Bristow AW Nichols WF Webb KS Conway B 《Rapid communications in mass spectrometry : RCM》2002,16(24):2374-2386
Mass spectral libraries provide a tool for identifying unknown compounds using both molecular weight and fragmentation information. Mass spectrometers with electrospray ionisation (ESI) and atmospheric chemical ionisation (ApCI) sources have the capability to produce data of this type using in-source collisionally induced dissociation (CID), and in-source CID libraries can be created. Due to the variation in electrospray source design from different instrument manufacturers, the production of reproducible in-source CID spectra that can be used in libraries for all instrument types is not a trivial task. To date, the evaluation of the production of in-source CID libraries has tended to focus on similar instruments from one manufacturer. The studies have also tended to focus on specific compound classes, with a limited molecular weight range.This report describes the findings from the investigation of protocols for the creation of mass spectral libraries using ESI in-source CID on six instruments from four different manufacturers. The overall goal was to create a spectral library for the identification of unknowns. The library could then be applied across all manufacturers' electrospray instruments.Two different experimental protocols were attempted. The first used a tuning compound to establish standard ESI source conditions, with fixed fragmentation potentials. The second involved the attenuation of the [M + H](+) ion to a known degree. A diverse range of compounds (pharmaceutical, photographic, pesticides) was tested to establish the reproducibility of the spectra on the six instruments. Both protocols produced spectra on the various instruments that in many cases were very similar. In other examples, the spectra differed not only in their relative ion abundances, but also in terms of the spectral content. Important observations regarding the effect of ion source design are also reported.The degree of spectral reproducibility was calculated off-line by comparing the five most abundant ions (20% for each ion that matches) from each spectrum on each instrument. This approach was adopted, as we do not possess a software package that met our requirements for spectral comparison. Match factors (% fit) were calculated by comparing each spectrum against the spectra recorded for the same compound and then for all other compounds, on each instrument. The % fit values derived by the off-line approach gave a clear view of the spectral reproducibility from instrument to instrument and also discriminated the spectra of the various compounds from each other. The applicability of this approach was tested using a blind trial in which several compounds were presented as unknowns, their in-source CID spectra recorded and the five-ion approach used for identification. 相似文献
34.
Taylor MJ Hunter K Hunter KB Lindsay D Le Bouhellec S 《Journal of chromatography. A》2002,982(2):225-236
A LC-MS-MS method capable of the quantitative determination of a range of pesticide residues present in crude extracts from a variety of fruit and vegetables has been developed. Isocratic LC conditions have been used in conjunction with electrospray ionisation tandem mass spectrometry to detect and identify up to 38 pesticides presented as various mixtures in different matrices. The utility of the method is demonstrated by the analysis of crude extracts, with no sample clean up, from grape, kiwi fruit, strawberry, spinach, lemon, peach and nectarine. Mean recoveries ranging from 63 to 96% with relative standard deviations < 20% were obtained for 30 of the 38 pesticides following analysis of organic produce fortified at concentrations between 0.01 and 0.8 mg/kg. Detected residues were quantified from interpolation against calibration data generated using matrix-matched standards that covered analyte concentration ranges between 0.005 and 0.8 microg/ml. Conditions suitable for the qualitative and quantitative confirmation of residues detected in samples are specified. 相似文献
35.
Bentley KW 《Natural product reports》2005,22(2):249-268
This review covers beta-phenylethylamines and isoquinoline alkaloids derived from them, including further products of oxidation, condensation with formaldehyde and rearrangement, some of which do not contain as isoquinoline system, together with napthylisoquinoline alkaloids, which have a different biogenetic origin. The occurrence of the alkaloids with the structures of new bases, together with their reactions and syntheses, are reported. The literature from July 2003 to June 2004 is reviewed, with 145 references cited. 相似文献
36.
The synthesis of the eight-membered ring containing two disulfides, 1,2,5,6-tetrathiacyclooctane, is described. It is characterized by x-ray crystallography as well as by mass, IR, Raman, 1H-NMR und UV spectroscopy 相似文献
37.
The total synthesis of tetrahydroisoquinoline alkaloids (+/-)-renieramycin G (4) and a lemonomycinone analogue (7) is described. A general strategy to synthesize both the mono- and bistetrahydroisoquinoline alkaloids from a common advanced intermediate, 17, is presented. 相似文献
38.
Terence C. Gibb Robert Greatrex Norman N. Greenwood Kenneth G. Snowdon 《Journal of solid state chemistry》1975,14(2):193-202
The magnetic and structural properties of the solid solution SrFexRu1?xO3?y (0 ? x ? 0.5) have been studied using 57Fe and 99Ru Mössbauer spectroscopy and other techniques. These phases, which are here reported for the first time, have a distorted perovskite structure. The iron substitutes exclusively as Fe3+ and thereby causes oxygen deficiency, but has little effect on the magnetic behaviour of the Ru4+ until x > 0.2, whereupon the metallic band system begins to revert to a localized electron structure. The properties of a sample with x = 0.3 are complex and intermediate in character. For x > 0.3 the oxygen deficiency is reduced by substantial oxidation to Ru5+ until at x = 0.5 the system corresponds to Sr2Fe3+Ru5+O6. 相似文献
39.
4-(4-Hydroxyphenyl)-2-phenylamino-1,8-naphthyridine was prepared via cyclisation of N-phenyl-N′-3-(4-hydroxyphenethen-1-yl)pyridin-2-ylthiourea in the presence of mercuric oxide. Derivatives of 4-methyl-2-aminoquinolines were prepared in a similar manner from 2-vinylphenylthioureas. 相似文献
40.
The molecular structures of 1,3-benzodioxole and 1,3-indandione partially oriented in nematic solvents have been studied by NMR. Results for 1,3-indandione agree well with a planar model. The structural parameters are similar to those obtained by X-ray studies. No keto-enol tautomerism is observed. An anomalous structural result is obtained for 1,3-benzodioxole if the molecule is assumed to be planar. Dipolar couplings agree well with puckered model. The puckering angle is found to be about 15.5° ± 2°, similar to the values observed for TTF, TSeF and 2,5-dihydrofuran. 相似文献