c and under an argon atmosphere a solution of tertiary amyl alcohol 20 mmols in 5 ml tetrahydrofuran stirring was continued for 2 hrs during which time the liquid became black an additional portion of tertiary amyl alcohol 32 mmol was then added to neutralize the remaining sodium hydride and the mixture was allowed to return to room temperature a non pyrophoric black suspension resulted which was then transferred under argon to a parr model 4561 300 ml stirred pressure reactor containing 1 3 g molybdenum hexacarbonyl 5 mmol to which an additional 70 ml tetrahydrofuran was added after flushing with hydrogen the reactor was charged with 300 psi of a mixture of 33 carbon monoxide in hydrogen and heated to 100 u00b0 c the pressure decreased during the run due to syngas consumption during this time the catalyst precursor was 34 conditioned 34 that is converted to the active catalyst after 2 hr the pressure had decreased to 50 psi and the reactor was cooled it was then recharged with syngas to 300 psi heated again to 100 u00b0 c and similar gas consumption was observed after a third charging and heating cycle the reactor was cooled and a sample was withdrawn and analyzed the total gas charge was 300 mmol with a total pressure drop equivalent to 270 mmol gas usage gas chromatographic analysis of the liquid showed 67 mmol methanol was produced no methane or carbon dioxide was found in the gas phase this amounts to about 74.