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The 1,2-azaphosphinine, 9 , and the 1,3-diphosphinine, 10 , can be isolated from a mixture resulting from the reaction of 1,1,3,3-tetrakis(dimethylamino)-1λ5,3λ5-diphosphete, 1 , and ethyl isothiocyanate. The reaction of 1 with phenyl isothiocyanate yields the 1,2-azaphosphinine, 16 . Mechanisms for the formation of the compounds 9 , 10 , and 16 are suggested. The properties, the NMR, mass, and IR spectra, and the molecular and crystal structures of 9 and 10 are described and discussed. 相似文献
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Alfred Schmidpeter Peter Mayer Johanna Stocker Kenneth A. Roberts Peter J. Stang 《Heteroatom Chemistry》1991,2(5):569-573
One example each is given for the reaction of bromoacetylenes and ethynyl-phenyliodonium tosylates with bis(diphenyl phosphino)methane. The yellow crystalline 1:1-addition products are diphospholium salts. They readily and selectively hydrolyze to give 2-phosphinoylethenyl phosphonium salts. 相似文献
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Synthesis of Fluoro-λ5-monophosphazenes and Fluoro-1,3-diaza-2λ5,4λ5-diphosphetidines by Means of the Staudinger Reaction 35 Tetrafluoro- and 2 difluorodiaza-diphosphetidines as well as 4 difluoro- and 30 monofluoro-λ5-monophosphazenes were prepared by the Staudinger reaction between tervalent phosphorus fluorides, RnPF3?n (n = 1, 2; R = R2N, (CH2)5N, O(CH2)4N, RO, (CH2O)2, alkyl, aryl) and phenylazides, X? C6H4N3 (X = H, 4-CH3, 4-Cl, 4-Br, 4-NO2, 3-NO2). PF3 does not react with phenylazide The influence of substituents on the structure of the reaction products is discussed. Kinetic measurements allowed to determine the constants λPI of the substituents (CH2)5N, O(CH2)4N and R(C6H5)N (R = CH3, C2H5, n-C4H9). 相似文献
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Haiko Beckmann Gisela Ohms Gisbert Großmann Kerstin Krüger Klaus Klostermann Volker Kaiser 《Heteroatom Chemistry》1996,7(2):111-118
From the crude product of the synthesis of the dithiadiphosphetane [RP(S)S]2 (with R = 2,4,6-iPr3C6H2), the trans-oxathiadiphosphetane has been isolated, C30H40OP2S3. X-ray structure analysis and mass spectroscopic investigations give unequivocal evidence for this structure: monoclinic, C2/c (no. 15), a = 13.066(8), b = 21.726(8), c = 12.070(6) Å, β = 103.54(10)°, V = 3331 Å3, Z = 4, and Dc = 1.158 g/cm3. The asymmetric unit consists of half the formula unit. Solid-state 31P NMR spectra give information about the chemical shift anisotropy. Results of IGLO calculations of the 31P nuclear magnetic shielding tensor agree satisfactorily with the experimental data. Monitoring the reaction of several dithiadiphosphetanes with benzophenone in solution by 31P NMR spectroscopy indicates that additional oxathiadiphosphetanes as well as thiotrimetaphosphonates are present. © 1996 John Wiley & Sons, Inc. 相似文献