Trichloro tripyridine molybdenum III

Trichloro (tripyridine) molybdenum (III) has been prepared by the reaction of molybdenum(III) chloride with pyridine at 270° for 5 hours in a sealed tube. The preparation described below using potassium hexachloromolybdate-(III) as starting material is carried out at a lower temperature, requires less time, and involves no special apparatus. 

To 50 ml. (about 0.6 mol) of reagent-grade pyridine in a 125-ml. round-bottomed flask there is added 8.5 g. (0.02 mol) of potassium hexachloromolybdate(III). The mixture is heated with a Glas Col mantle, or microburner, and refluxed at 115 to 117° for 3 hours using a conventional water-cooled reflux column. At the end of the reaction time, upon cooling, a yellow precipitate suspended in a dark brown solution is observed. 

Purification for purposes of elemental analyses is carried out by redissolving the precipitate in 40 ml. of pyridine and refluxing for 2 hours and then precipitating, washing, and drying as above. Removal of traces of water and pyridine is carried out by pistol drying under 10-mm. pressure at the reflux temperature of acetone, 57°. 

Trichloro(tripyridine)molybdenum(III) is a deep yellow solid, which decomposes at 172 to 182°, yielding free 

The compound is almost completely insoluble in hot or cold water, slightly soluble in 95% ethanol, benzene, and acetone, and soluble in methanol and glacial acetic acid. No solution is observed in hot or cold concentrated hydrochloric acid or in aqueous ammonia. It decomposes to give solutions in hot and cold concentrated nitric and sulfuric acids. In concentrated sodium hydroxide solutions, decomposition occurs on heating, with the formation of violet-black precipitates. 

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