Preparation of tervalent molybdenum complexes and a study of their reduction by zinc under low pressure of carbon monoxide
M'Thiruaine, Cyprian Muturia
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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.