In a
5-l. flask fitted with a
reflux condenser are placed
2.5 l. of 95 per cent ethyl alcohol and
340 g. (4.5 moles) of commercial (73–75 per cent) potassium hydroxide. The mixture is gently shaken until the hydroxide is dissolved, 1330 g. (1.5 l., approximately 4 equivalents) of rape-seed oil is added with shaking (Note
1), and the mixture is refluxed on a
steam bath for twenty-five to thirty hours.
The hot mixture is poured, with stirring, into 15 l. of warm water (50–60°), and is followed by
700 cc. (8.2 moles) of concentrated (36 per cent) hydrochloric acid (Note
2). After standing until the layers are distinct (ten to fifteen minutes), the lower layer is siphoned off as completely as possible and the oil is washed with two 1-l. portions of warm water.
The oil thus obtained, which should amount to 1460–1600 cc., is dissolved in three times its volume of
95 per cent ethyl alcohol and the mixture cooled to −10 to 0°, when the
erucic acid crystallizes (Note
3). After six to eight hours at this temperature, the crude
erucic acid is collected on a
basket centrifuge (Note
4). The mother liquor, on chilling, yields a second crop of
erucic acid. The combined product (
800–1100 g.) melts either partially or wholly at room temperature, owing to the presence of
oleic acid. It is dissolved in an equal volume of alcohol, chilled for six hours at 0°, and centrifuged as before, when it is obtained in well-defined crystalline form. The second crop of this recrystallization resembles that of the first crystallization and must again be recrystallized. The product is finally recrystallized once again from an equal volume of
95 per cent alcohol. The recrystallized acid contains alcohol, which is removed by heating to constant weight on the
steam bath under diminished pressure. The yield of acid is
260–360 g. (Note
5); the acid melts at
31–32° (Note
6).