Synthesis of a triazaphosphahomoadamantane

Abstract

peaks in the 31, 45, 59, 73, etc., series and can be used in low-resolution mass spectrometry to differentiate from the 43, 57, 71, etc., series of hydrocarbon peaks.Infrared spectra. The fundamental frequencies for related epoxides in the frequency range 2.5-8.0 µ were the same for all compounds. Henbest et al. (4) report specific C-H stretching bands in the range of 3050-2990 cm-1 for the epoxide function. We should have been able to determine these bands with the instrument used but were unable to detect them.The 1,2-epoxides substantiate data published by Shreve et al. (9) for the characteristic absorption pattern at 11.0 and 12.0 µ for the oxirane derivative of terminally unsaturated compounds. This pattern is eliminated as the epoxide moves closer to the center of the molecule. A single diagnostic peak Is shown for all the 2,3-epoxides at 11.7 µ, for all the 3,4epoxides at 11.3 µ, and for all the 4,5-epoxides between 11 and 11.2 µ.

Between Adamantane and Atrane: Intrabridgehead Interactions in the Cage‐Like Phosphane Related to a Novel Tris(homoadamantane) Ring System

“…Synthetic approaches to mono‐ and bicyclic ligands with the PTA‐like topology have also been explored . Several attempts intending to expand the triazacyclohexane ring of PTA have resulted in the synthesis of asymmetric cage‐like phosphanes, which were found to be chemically unstable . The counterpart of PTA with a symmetric 1,4,7‐triazacyclononane macrocycle incorporated into the cage has been recently synthesized in our laboratory .…”

Decomposition reactions of hydroxyalkylphosphorus compounds. I. Reaction of benzylbis(.alpha.-hydroxybenzyl)phosphine oxide with primary amines

“…The use of method b with p-nitroaniline produced only the diamine, 23, in a 47% yield. Attempts at recrystallization yielded lower melting products, so the original material was used as the analytical sample, 23: mp 195-196°; ir (KBr) 2.95 and 3.05 (NH), 3.25 (medium, aromatic CH), 6.25 (C=C), 6.67 and 7.55 (N02), 8.45 (P=0), 9.0 (? ), bands at 6.25, 6.67, 7.55, and 9.0 µ are all stronger absorptions than the phosphoryl; NMR (DMSO-de) 2.…”

“…-3.67 (m,9 H, contains PCH2, NCH2, CH3OCH2, and OCH3 spike at 3.36),3.95 (d, J = 18 Hz, 1 H, PCHN), 4.98 (d, J = 12 Hz, 1 H, PCHO), 6.90-7.67 (m, 15 H, aromatics); these assignments were made after D20 exchange, since the NH and OH protons were spread out along the base line at 2.4-5.4. Integration was decreased only in this region after exchange with D20.Anal.…”