Synthesis of Dimethyl Oxalate

Combine 64 g of anhydrous oxalic acid, 75 mL of dry methanol and 25 mL of conc. sulfuric acid in a beaker with vigorous stirring. Gently heat the solution to its boiling point, with plastic wrap on, then slowly cool down to room temperature. Put the solution into a freezer for 24 h, filter, refreeze and filter the filtrate. Dissolve the crystals in hot methanol, allow to crystallize in a freezer, filter and dry in a desiccator.

Source

Capture

The combined reagents were brought to the boiling point

ed

Cooling down

efd

Crude dimethyl oxalate crystallized out in the freezer

gh

Filtering the slush

rgs

The crude product was recrystallized from methanol

fg

Filtering the slush

jy

Pure dimethyl oxalate

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