In a
5-l. round-bottomed flask, fitted with a stopper carrying a
long reflux condenser, a
mechanical stirrer (Note
1), and a
separatory funnel, are placed 2 l. of water (Note
2),
1 kg. (4.95 moles) of trimethylene bromide (p. 30) (Note
3), and
370 g. (3.9 moles) of phenol. The stirrer is started, and the mixture is heated to boiling. To the boiling solution is added a solution of
150 g. (3.75 moles) of sodium hydroxide in 500 cc. of water at such a rate that all is added in about one hour. The mixture is refluxed for five to six hours longer to complete the reaction, then cooled, and the upper water layer is separated and discarded.