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A cyclotriphosphazene bearing two 4-oxypyridine groups on the same phosphorus atom, gem-[N(3)P(3)(O(2)C(12)H(8))(2)(OC(5)H(4)N-4)(2)] (I), and its analogous polymer [{NP(O(2)C(12)H(8))}(0.7){NP(OC(5)H(4)N-4)(2)}(0.3)](n) (II), have been used to prepare gold or silver, cyclic and polymeric, metallophosphazenes. The following complexes, gem-[N(3)P(3)(O(2)C(12)H(8))(2)(OC(5)H(4)N-4{ML})(2)] (ML=Au(C(6)F(5)) (1) or Au(C(6)F(5))(3) (2)), [N(3)P(3)(O(2)C(12)H(8))(2)(OC(5)H(4)N-4{AuPPh(3)})(2)][NO(3)](2) (3), and [N(3)P(3)(O(2)C(12)H(8))(2)(OC(5)H(4)N-4{AgPPh(2)R})(2)][SO(3)CF(3)](2) (R=Ph (4) or Me (5)) have been obtained. Complexes 1 and 4 are excellent models for the preparation of the analogous polymers [{NP(O(2)C(12)H(8))}(0.7){NP(OC(5)H(4)N-4{ML})(2)}(0.3)](n) (ML=Au(C(6)F(5)) (P1), Ag(OSO(2)CF(3))PPh(3) (P2)). All complexes have been characterized by elemental analysis, various spectroscopic methods, and mass spectrometry. The polymers were further investigated by thermochemical methods (thermogravimetric analysis) and differential scanning calorimetry. For compounds 1-5 and for the starting phosphazene I, a mixture of different stereoisomers may be expected. The stereochemistry in solution has been studied by variable-temperature NMR spectroscopy studies, which provided evidence for interconversion processes that involve changes in the chirality of a 2,2'-dioxybiphenyl group. A single-crystal X-ray analysis of the gold complex 2 confirmed not only the proposed structure, but also S,S and R,R configurations at the two biphenoxy-substituted phosphorus centers, in contrast to those observed for the precursor I. Pyrolysis of these new metallophosphazenes was also studied. Notably, pyrolysis of the gold derivatives gave macroporous metallic gold sponges without the requirement of either an external reducing agent or a porous support. These materials were all characterized by XRD, TEM, SEM, and energy-dispersive X-ray spectroscopy.
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PMID:Metallocyclo- and polyphosphazenes containing gold or silver: thermolytic transformation into nanostructured materials. 1990 39

Silver nanoparticles have been prepared from a chemical reduction approach and supported on modified TEOS (tetraethylorthosilicate) xerogels to be studied as a nanocatalyst in the conversions of benzopyranopyrimidines (with primary as well as secondary amines along with the mechanism by trapping the imine intermediate) and also in the synthesis of gem-bisamides. Different conditions for the performance of the nanocatalyst have been screened and tolerance with respect to variable functionalities has been observed, resulting in excellent yields; and confirmation of products synthesized has been done using studies like 1H NMR, 13C NMR and mass analysis. Also, SEM-EDX and TEM of the nanocatalyst have been performed to know the internal and external morphology, size and elemental composition. UV and XRD analysis to confirm the silver nanoparticles' and xerogel's presence, TGA to study the thermal stability and FTIR to study the modification pattern of the nanocatalyst have been undertaken and presented in this work.
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PMID:A nano silver-xerogel (Ag nps@modified TEOS) as a newly developed nanocatalyst in the synthesis of benzopyranopyrimidines (with secondary and primary amines) and gem-bisamides. 2851 92