A mixture of 105.6 g. (1.1 moles) of freshly distilled furfural, 87.0 g. (1.0 mole) of 98% cyanoacetic acid (Note 1), 3.0 g. of ammonium acetate, 200 ml. of toluene, and 110 ml. of pyridine is placed in a 1-l. round-bottomed flask equipped with a Stark and Dean water trap and reflux condenser. The mixture is boiled under reflux for 2 days. The theoretical quantity of water is collected in the trap within 1 hour. Upon completion of the reflux period, the solvent is removed under reduced pressure by heating on a water bath. The residue, distilled through a 15-cm. Vigreux column at 11 mm. pressure, yields 88.6–93.3 g. (74.5–78%) of colorless liquid boiling at 95–97°, n²⁵D 1.5823–1.5825.