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Anodic oxidation of 1′,8′-dimethyl- and other 1′,8′-disubstituted a.c -biladiene salts affords novel cyclized products. In addition to porphyrin, an unconjugated macrocyclic intermediate product resulting from oxidadve cyclizatfon during porphyrin synthesis is isolated, structurally identified, and characterized with regard to its spectroscopy, electrochemical behavior and chemical reactivity. The formation of a novel homoporphyrin from a 1′-ethoxycarbonylmethy-8′-(2-methoxycarbonylethyl)- a,c -biladiene salt is also briefly discussed.

Phosphosilicate molecular precursor for the synthesis of NASICON, natrium super ionic conductor, Na1+xZr2SixP3−xO12 (x = 1 and 2) has been devised and prepared by the hydrolysis of tetraethoxysilane (TEOS) employing sodium phosphate solution. The molecular precursor was reacted with Zr(OC3H7)4 in ethanol under solvolytic condition to yield nano precursor material of NASICON. This material was annealed at high temperature to yield phase-pure NASICON. The molecular precursor was characterized using 31P NMR, FTIR spectral data, powder XRD pattern and TG/DTA studies. The structure of the molecular precursor was deduced from the powder XRD data, which indicates the presence of edge sharing tetrahedral arrangement of −O−Si−O−P−O−Si− chain. The NASICON precursor material was characterized using TG/DTA, FTIR, TEM, SEM, MAS 31P NMR and XRD. The conductivity of the synthesized NASICON material was measured using the pellet annealed at 900 °C and was found to be 5.5 x10−3 S cm−1. The details on the preliminary inves...

8 We acticipate that this reaction, while quite useful in its own right, may also be the prototype for other novel transformations based on transition-metal-centered radicals.'* As a first step in this direction we plan to explore intermolecular additions of epoxides to activated olefins. Supplementary Material Available: Details of isolation and characterization (13C NMR, 'H NMR, HRMS, elemental analysis) of products 1-8 (4 pages). Ordering information is given on any current masthead page.