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A 5mL conical vial containing a magnetic spin-vane, equipped with a Hickman still and condenser, is charged with the following: 30 mg of p-toluenesulfonic acid monohydrate catalyst; 400 uL (412 mg) of ethyl acetoacetate; 200 uL (222mg) of ethylene glycol; and 2.0 mL of anhydrous toluene.
Use a micropipet to dispense each liquid.
Heat the reaction mixture in a pre-stabilized sand bath (~140C) and maintain a vigorous reflux for 30 minutes
As the reaction progresses, the water formed is separated from the solution by azeotropic distillation with the toluene.
The water then separates from the toluene on cooling in the upper portion of the Hickman still and collects on the walls and in the collar while the toluene returns to the distillation flask.
The vial is then cooled to room temperature and the toluene solution extracted with 1.0 Ml of 1M aqueous NaOH solution followed by two 1mL portions of water.
During each extraction, the aqueous solution is added and the vial is capped and then gently shaken.
After separation of the layers, the cap is removed and the aqueous layer separated and discarded.
The remaining toluene solution is now dried by passing through a 3-4cm column of anhydrous sodium sulfate in a Pasteur pipet...