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1.
混合三烃基锡衍生物的研究——Ⅷ.甲基二环己基锡(取代)苯氧乙酸酯的合成、结构表征和生物活性 总被引:1,自引:0,他引:1
杨志强 谢庆兰单书香本文合成了二十个混合甲基二环己基锡取代苯氧乙酸酯.研究了这些化合物的IR,NMR(~1H,~(13)C,~(119)Sn),结果表明,除邻甲氧基苯氧乙酸酯外,这些化合物都可能是以羰基氧为桥连的五配位聚合有机锡化合物.~(119) Sn NMR的研究结果表明,~(119)Sn化学位移与苯环上取代基有一线性关系:~(δ119)Sn=6.23σ+94.67,r=0.943.农药的初筛表明,这些化合物除有很好的杀螨活性外,还有一定的杀菌,除草和植物激素作用. 相似文献
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三苄基锡羧酸酯的合成及其结构表征 总被引:16,自引:0,他引:16
本文以(三苄基锡)氧化物和相应的羧酸反应, 合成了20个三苄基锡羧酸酯, 由波谱对结构的研究表明, 红外光谱的酰基振动频率与羧基上取代基的空间和电子效应密切相关, 三苄基锡羧酸酯的结构微小变化, 明显地反映了^1^1^9Sn和^1^3CNMR化学位移的差异, ^1^1^9Sn化学位移与三苄基锡取代的苯甲酸酯的对位取代基Hammett常数(σ)之间存在着良好的线性关系: δ~1~1~9~S~n=15.48σ+14.23, n=7, r=0.995, 去烃基化是这一类化合物质谱裂解的特点。 相似文献
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本文合成了二十个混合甲基二环己基锡取代苯氧乙酸酯。研究了这些化合物的IR, NMR (^1H, ^1^3C, ^1^1^9Sn), 结果表明, 除邻甲氧基苯氧乙酸酯外, 这些化合物都可能是以羰基氧为桥连的五配位聚合有机锡化合物。^1^1^9Sn NMR的研究结果表明, ^1^1^9Sn化学位移与苯环上取代基有一线性关系: δ^1^1^9Sn=6.23σ+94.67, r=0.943。农药的初筛表明, 这些化合物除有很好的杀螨活性外, 还有一定的杀菌, 除草和植物激素作用。 相似文献
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本文合成了二十个混合甲基二环己基锡取代苯氧乙酸酯。研究了这些化合物的IR, NMR (^1H, ^1^3C, ^1^1^9Sn), 结果表明, 除邻甲氧基苯氧乙酸酯外, 这些化合物都可能是以羰基氧为桥连的五配位聚合有机锡化合物。^1^1^9Sn NMR的研究结果表明, ^1^1^9Sn化学位移与苯环上取代基有一线性关系: δ^1^1^9Sn=6.23σ+94.67, r=0.943。农药的初筛表明, 这些化合物除有很好的杀螨活性外, 还有一定的杀菌, 除草和植物激素作用。 相似文献
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取代基对1,4-双[β-(4-取代苯基)乙烯基]苯化合物红外光谱的影响 总被引:1,自引:0,他引:1
取代基对红外光谱特征频率的影响曾有报导,但对1,4-双[β-(取代苯基)乙烯基]苯类化合物还未曾研究。我们测试了它们的红外光谱,发现取代基常数σ_p、σ_p~o及σ_p~ 与反式烯键上碳—氢键的面外变角振动频率δ=C-H(面外)之间存在一定线性关系。 相似文献
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Beltrán HI Zamudio-Rivera LS Mancilla T Santillan R Farfán N 《Chemistry (Weinheim an der Bergstrasse, Germany)》2003,9(10):2291-2306
Twenty-four 2,2-di-n-butyl- and 2,2-diphenyl-6-aza-1,3-dioxa-2-stannabenzocyclononen-4-ones, each having a transannular N-->Sn bond, have been prepared by one-step reactions of alpha-amino acids (1 a-l), salicylaldehyde (2), and either di-n-butyltin(IV) oxide (3) or diphenyltin(IV) oxide (4). The new methodology constitutes an easy, highly efficient one-step synthesis of diorganotin(IV) derivatives, such as 5 a-l and 6 a-l, from iminic tridentate ligands without isolation of the Schiff bases. The structures of all the compounds have been established by a combination of (1)H, (13)C, (15)N, and (119)Sn NMR spectroscopy, IR spectroscopy, mass spectrometry, and elemental analysis. In all cases, the (119)Sn chemical shifts, as well as the (1)J((119)Sn,(13)C) coupling constants, are indicative of pentacoordinated tin atoms in solution. The structures of compounds 5 a, d, f, 6 a, b, b-racemic, c, d, f, g, and l have been established by single-crystal X-ray diffraction analyses. The tin atoms in 5 d, f, 6 a, b, b-racemic, c, d, g, and l each have a distorted trigonal-bipyramidal (TBP) geometry, with the oxygen atoms from the phenol and carboxylate moieties occupying the axial positions, and the imine nitrogen and phenyl or n-butyl substituents occupying the equatorial positions. Compounds 5 a and 6 f show distorted octahedral (DOC) geometries due to intermolecular coordination of the carbonyl oxygen to the tin atom, in a trans disposition to the N-->Sn bond, leading to trimeric 5 a and a polymeric structure for compound 6 f. Additionally, measurement of the one-bond coupling constants (1)J((119)Sn,(13)C) in diphenyltin(IV) complexes (6 a-l) and their correlation with the CSn-C bond angles has allowed the derivation of an equation that can be applied to assess the geometry around the tin atom for other diphenyltin(IV) compounds in solution. 相似文献
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A complete series of diphenyl and mixed methyl/chlorine/bromine/iodinephenyl substituted oxadithia- and trithiastannocanes has been prepared by reactions between the respective disodium dithiolates and tin dihalides. The 13C NMR chemical shifts of these compounds and the coupling constants J(119Sn13C) are dependent upon the magnetic anisotropy of the substituents and the bond angles at the tin atom. The crystal structure of 2,2-diphenyl-1,3,6-trithia-2-stannocane has been determined and refined to R = 0.039. The environment of Sn is a monocapped tetrahedron (transannular distance Sn?S 324.6(1) pm). This type of coordination, intermediate between a tetrahedron and a trigonal bipyramid, is discussed quantitatively and compared with a series of analogous compounds. The eight-membered ring has the boat-chair conformation. 相似文献
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Stephen J. Blunden Robin Hill John N.R. Ruddick 《Journal of organometallic chemistry》1984,267(2):c5-c8
Bis(tributyltin) oxide or trimethyltin hydroxide react with carbon dioxide to afford the bis(trialkyltin) carbonates, (R3SnO)2CO; 119Sn NMR (in the case of R = Bu) or 119mSn Mössbauer spectroscopy show that these compounds contain 4- and 5-coordinate tin atom sites. 相似文献
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Centineo G Rodríguez-González P Blanco González E García Alonso JI Sanz-Medel A 《Journal of mass spectrometry : JMS》2004,39(5):485-494
The development of a rapid, precise and accurate speciation method for the simultaneous determination of mono-, di- and tributyltin in environmental samples is described. The method is based on using isotope dilution gas chromatography/mass spectrometry (GC/MS) with electron ionization, a widely used technique in routine testing laboratories. A mixed spike containing (119)Sn-enriched monobutyltin (MBT), dibutyltin (DBT) and tributyltin (TBT) was used for the isotope dilution of the samples. Five molecular ions were monitored for each analyte, corresponding to the (116)Sn, (117)Sn, (118)Sn, (119)Sn and (120)Sn isotopes. The detection at masses corresponding to (116)Sn and (117)Sn were used to correct for m + 1 and m + 2 contributions of (13)C from the organic groups attached to the tin atom on the (118)Sn, (119)Sn and (120)Sn masses with simple mathematical equations and the concentrations of the butyltin compounds were calculated based on the corrected (118)Sn/(119)Sn and (120)Sn/(119)Sn isotope ratios. The (119)Sn-enriched multispecies spike was applied with satisfactory results to the simultaneous determination of MBT, DBT and TBT in three certified reference materials: two sediments, PACS-2 and BCR 646, and the mussel tissue CRM 477. The method was compared with a previously published GC/inductively coupled plasma MS isotope dilution procedure, developed in our laboratory, by injecting the same samples into both instruments. Comparable analytical results in terms of precision and accuracy are demonstrated for both atomic and molecular mass spectrometric detectors. Thus, reliable quantitative organotin speciation analysis can be achieved using the more widespread and inexpensive GC/MS instrument. 相似文献
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二氯马来酰亚胺有机锡化合物的合成和结构表征 总被引:4,自引:2,他引:2
合成了14个1-三羟锡基-3,4-二氯马来酰亚胺有机锡化合物,研究了它们的核磁共振谱(^1H,^13C,^119Sn),外光谱质谱,并且得出,锡原子上的烃基对化合物的生物活性有很大的影响。 相似文献
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Junzo Otera 《Journal of organometallic chemistry》1981,221(1):57-61
119Sn chemical shifts, δ(119Sn), relative to Me4Sn in five- and six-coordinate organotin chelates were measured by means of FT NMR spectroscopy. 119Sn resonances were found to lie between ca. ?90 and ?330 ppm in the five-coordinate compounds and between ca. ?125 and ?515 ppm in the six-coordinate derivatives. thus δ(119Sn) moves upfield by 60–150 ppm with a change of the coordination number of tin from four to five and by 130–200 ppm from five to six. the δ(119Sn) values were shifted depending on the nature of chelating ligands and this shift was discussed in terms of the bonding between the ligand and tin. Replacement of methyl groups attached to tin by phenyl groups in five- and six-coordinate compounds induces upfield shifts in δ(119Sn) parallel to those found in four-coordinate organotin halides. 相似文献
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Jens Klein Frank Thunecke Rolf Borsdorf 《Monatshefte für Chemie / Chemical Monthly》1992,123(8-9):801-806
Summary Eleven compounds have been prepared by azeotropic destillation of water from toluene solutions of bis(tri-n-butyltin)oxide and N-acetyl amino acids. All derivatives are white solids.119Sn-NMR-spectra of the tri-n-butyltin compounds have been studied in coordinating and non coordinating solvents. The chemical shifts and the coupling constants1
J(119Sn,13C) depend significantly on the coordination number of the tin atom and on the properties of the substituents. The data for the compounds are discussed in comparison with those for other tri-n-butyltin compounds. 相似文献
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本文合成了13种三苯基锡-O,O-二芳基二硫代磷酸酯,测定了它们的IR、~1H、~(31)C、~(119)SnNMR,MS和元素分析,结果表明该类化合物具有单体的四面体四价锡结构。 相似文献