A solution containing 140g glycine ethyl ester hydrochloride (1mol) in 250ml water is placed in a 2L four- neck flask. 600 ml dichloromethane is added and the mixture is cooled to -5ºC under a nitrogen atmosphere. A solution containing 83g sodium nitrite in 250ml water is cooled to 0ºC and added with stirring to the reaction mixture. While keeping the reaction temperature below -9ºC, 95g 5% sulfuric acid is added dropwise to the reaction over a 3 minute period. After ten minutes addition stirring the reaction is transferred to a 2L separatory funnel while cold. The isolated yellow-greenish organic phase is poured into a cooled 1L 5% sodium carbonate solution, then placed into a separatory funnel and shaken. The isolated aqueous phase is extracted with 75ml dicholoromethane, dried over 15g anhydrous sodium sulfate, and concentrated under reduced pressure (350mmHg). Futher concentration at 20mmHg and a bath temperature of 35ºC gives 90 ~ 100g (79 ~ 80%) yellow oily substance.
The product is pure enough to be used for ordinary synthesizing purposes. It is explosive, and distillation under even reduced pressure is hazardous.
*Ethyl diazoacetate is explosive and very toxic. Wear protective gloves, protective goggles, protective mask, and use a safety screen. Work in a well ventilated fume hood.
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