In a
2-l. round-bottomed flask fitted with a
reflux condenser protected by a
calcium chloride tube,
11.5 g. (0.5 gram atom) of finely cut sodium is dissolved in 250 cc. of absolute alcohol. To this solution is added
80 g. (0.5 mole) of ethyl malonate followed by
30 g. (0.5 mole) of dry urea dissolved in
250 cc. of hot (70°) absolute alcohol. After being well shaken the mixture is refluxed for seven hours on an
oil bath heated to 110°. A white solid separates rapidly. After the reaction is completed, 500 cc. of hot (50°) water is added and then enough
hydrochloric acid (sp. gr. 1.18) to make the solution acidic (about 45 cc.). The resulting clear solution is filtered and cooled in an
ice bath overnight. The white product is collected on a
Büchner funnel, washed with 50 cc. of cold water, and then dried in an
oven at 105–110° for three to four hours. The yield of
barbituric acid is
46–50 g. (
72–78 per cent of the theoretical amount).