Preparation of tervalent molybdenum complexes and a study of their reduction by zinc under low pressure of carbon monoxide

Abstract

Previously, molybdenum hexacarbonyl, MO(CO)6 has been prepared by reduction of high oxidation state molybdenum compounds such as MOCl5 under high pressure (60-100 atm.) and temperature (20-100°C), carbonylation of metal oxide at very high pressure (2000 atm) and temperature (300°C) or carbonylation of the metal itself at 250 atm pressure and 200°C. Products made under these conditions are very expensive. The present study was aimed at investigating whether MO(CO)6 can be prepared under mild conditions by reducing trihalotris(tetrahydrofuran)molybdenum(III), Mo(THF)3X3 (X=C1, Br) with zinc dust at I to 2 atmospheres. The results confirm beyond any reasonable doubt that this is possible. Products were isolated using thin layer and column chromatography, and identified using infrared spectroscopy and elemental analysis.