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Reiter SA, Nogai SD, Schmidbaur H: Synthesis and auration of primary and di-primary heteroaryl-phosphines. Dalton Trans. 2005 Jan 21;(2):247-55. Epub 2004 Dec 7.
Convenient high-yield syntheses of the primary and di-primary heteroaryl-phosphines R-PH2 and H2P-R'-PH2 (with R = 2-thienyl, 2-furyl, and R'= 2,5-thiophenediyl, 2,5-furandiyl, respectively) are presented. The products and a set of precursor molecules have been characterized by analytical and spectral data, and the crystal structures of selected molecules have been determined: 2-C4H3O-PCl2, 2,5-(Cl2P) 2C4H2O, 2,5-[(Et2N) 2P] 2C4H2E (with E = O, S). In the crystals, the two molecules with -PCl2 substituents adopt trans conformations, while the other two have the -P (NEt2) 2 groups rotated into a twist conformation. The reaction of the thienyl compounds with tris [(tert-phosphine) gold] oxonium tetrafluoroborates gave almost quantitative yields of the tri- and hexanuclear gold complexes, respectively: {2-C4H3S-P [Au (PR3)] 3}+BF4- and [2,5-{[(R3P) Au] 3P}2C4H2S] 2+(BF4 (-) 2, (R =tBu, Ph). The structures of the compounds with R3P =tBu3P ligands have been determined. In both cases the [2-C4H3/2S-P] units cap triangles of gold atoms in an array that can be described as three [Au (PR3)]+ cations bridged by a phosphido dianion (RP) 2-. |
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