An experimental attempt to synthesize methyl iodide by reacting iodine with methanol in the presence of aluminum foil. They used 40 g iodine and about 4.5 g aluminum foil formed into balls, with 50 mL methanol in a 250 mL flask equipped with a reflux condenser, ice-cold cooling water, and an aquarium pump to manage the exotherm. The reaction began after the aluminum oxide layer was removed by stirring; it was exothermic, with methanol condensing and signs of methyl iodide formation. The reaction was run for about an hour before reorganizing the setup for distillation to remove excess methanol and the product. Distillate was collected into an ice-cooled receiving flask with the condenser similarly cooled, and the crude product was dried with calcium chloride. The isolated product was a crude methyl iodide (14.6 g), estimated at a 33% yield relative to the starting iodine, significantly lower than the ethanol-based method. They speculated that methyl iodide may have escaped through the condenser or that the reaction is more water-sensitive, or that the aluminum foil method is less effective for methanol. They suggested skipping the reflux and distillation in a future run and ensuring an even drier setup, but warned yields would likely remain modest.
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