Synthesis of Diethyl Oxalate

To a reflux apparatus add 74 g of anhydrous oxalic acid and 200 mL of dry ethanol, reflux for 4 h. Cool down and set up for a distillation, discard ethanol which comes off at 80°C, discard water which comes off at 100°C, collect the diethyl oxalate which comes off at 160-170°C. Prepare 40 mL of conc. a solution of sodium chloride add it to separatory funnel then add the distillate too to the separatory funnel. Discard the bottom layer, dry the diethyl oxalate with anhydrous calcium chloride.

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The solution after 4h of reflux

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The crude diethyl oxalate after distillation

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Washing with conc. sodium chloride solution and collect the upper layer.

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