B.
DL-Aspartic acid. A mixture of
383 g. of the above crude product,
1 l. of concentrated hydrochloric acid,
1 l. of glacial acetic acid, and 1 l. of water is boiled under reflux in a
5-l. round-bottomed flask for 2–3 hours. The reflux condenser is then replaced by a
fractionating column, and the mixture is slowly distilled until the temperature at the head of the column has risen to 108°. This requires about 13 hours. The distillate amounts to 1.5 l.
(Note 3).
The residual mixture is allowed to cool, and the
phthalic acid which crystallizes is removed by filtration and washed with
350 ml. of 1% hydrochloric acid (Note 4). The combined filtrate and washings are distilled nearly to dryness on a steam bath under reduced pressure; the bulk of the hydrochloric and acetic acids remaining is removed by slowly adding 300 ml. of water through a
dropping funnel while the distillation under reduced pressure is continued. The dark brown residue is warmed on a steam bath with 700 ml. of water, is allowed to cool, and is filtered to remove a small amount of black insoluble matter. The filtrate is decolorized with
2 g. of Norit, 200 ml. of hot water being used to wash the
Norit. The volume of the combined filtrate and washings, amounting to about 1.2 l., is measured accurately, and a small portion is analyzed for chloride
(Note 5). An amount of
pyridine corresponding exactly to the chloride content is added, diluted with
500 ml. of 95% ethanol. The
DL-aspartic acid, which crystallizes at once, is separated by filtration after the mixture has stood for 24 hours at room temperature and is washed with 50–100 ml. of cold water
(Note 6).