Synthesis of Methyl Iodide from Iodine and red phosphorus Iodination

Add 60 mL of methanol and 75 g of iodine to a RBF, put the RBF in an ice bath with magnetic stirring and start adding 15 g of red phosphorus in 1-2 g portions. Keep the temperature below 40°C. Then start to distill with a hot water bath, when no more of distillate comes off stop heating. Pour the distillate into a separatory funnel and add 20 mL of conc. sodium chloride with few grams of sodium thiosulfate solution, shake, discard the aqueous layer then wash with 40 mL of water, discard the aqueous layer. Dry with anhydrous calcium chloride. Store in cold with copper wire to stabilize it.

Source

Capture

Adding the phosphorus slowly

ty

Al of the iodine dissolved and temperature raised

yujh

Distillation

rtgf

Crude methyl iodide

rfd

Washing with the sodium chloride thiosulfate solution

rgfs

Removing water with anhydrous calcium chloride

rgd

Pure methyl iodide

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