1-Oxo-4-hydroxymethyl-2,6,7-trioxa-1-phosphabicyclo[2.2.2]octane was oxidized with concentrated nitric acid to the corresponding acid. From the reaction of the acid chloride with various phenols and aryl amines, new bicyclophosphates, e.g. I (R = H, halo, alkyl, NO2, MeO; X = O, NH) were prepared The reduction of I (R = 2-NO2, X = O) with iron powder in HOAc gave the O甆 acyl migration product I (R = 2-OH, X = NH). The elemental anal., IR, 1H NMR, and MS spectra of these new compounds were recorded, and the crystal structure of I (R = 4-MeO, X = NH) was determine by the x-ray diffraction method.

Key words: VANADATE, AMMONIUM COMPOUND, CRYSTAL STRUCTURE DETERMINATION, X-RAY DIFFRACTION ANALYSIS, NITRIC ACID, REARRANGEMENT REACTION, BICYCLOOCTANE, OXYGEN HETEROCYCLICS, CLUSTER COMPOUND, PESTICIDES