Wanda Wojciechowska

Facile Preparation of Oxodiperoxymolybdenum(Pyridine)(Hexamethylphosphoric Triamide) (MoOPH)

Abstract The title compound is known and used as an oxidizing agent. The most useful application of it is the oxidation of the carban-ions obtained from esters, lactones, ketones, nitriles, aldehydes, sulphones and amides in order to obtain the hydroxy derivatives. The known method of synthesis of MoOPH involves the oxidation of MOO3 obtain to MOO5 with 30% hydrogen peroxide. We tried to MOO5 according to procedure described by Vedejs and unfortunately about 50% of the unreacted MOO3 had t o be filtered off from the MOO5 solution after 3.5 h. stirring at 40°C, so the yield of MOO5 HMPTH 0 was about 30%. We needed a bigger amount of title reagent and we started from molybdic acid monohydrate instead of MOO3 and 30% hydrogen peroxide. The reaction appeared slightly exotherrnic and took place in half an hour at 4O°c. All molybdic acid was dissoled and gave a yellow clear solution of Moo5. Addition of equimolar amount of HMPT gave the required MOO5HMPTH2O complex as a fine yellow crystalls in 61.9% yield. The...