Scientific American Supplement, No. 447, July 26, 1884 — John Shaqi
Scientific American Supplement, No. 447, July 26, 1884Various
Science
Scientific American Supplement, No. 447, July 26, 1884
Various
Science -- Periodicals
If we do not wish to utilize this crude substance at once, it will be
necessary to melt it in the water bath and pour it into a bottle under
close seal, where it will at once crystallize and solidify. If it
remains exposed to the atmosphere, it will soon become sticky and
turn partly into resin. Six kilos of lupuline, which included a large
proportion of sand, furnished 400 grammes of crude hop-bitter acid. The
first experiments in crystallization with petroleum ether gave poor
results; it is difficult to produce the acid pure in large quantities
by this process, as a small quantity of the above substance obstinately
clings to it, and it readily assumes a non-crystallizable form. Our
object is more readily attained if we crystallize it once from alcohol,
for which purpose we dissolve it in a little lukewarm alcohol, then
quickly cool the solution; flakes of a fatty substance will be
separated, which are removed by filtration with the aid of a
suction-pump. Then we throw a few small crystals of the acid into the
solution, and after a short time crystallization commences. As soon as
it appears to be ended, the mother solution is removed with the aid of a
platinum cone, and the crystals washed with a little cold alcohol. The
alcoholic mother solution, which still contains the chief part of the
bitter acid, must be quickly evaporated, and the residue consigned to
a flask. The acid crystallized from the alcohol is then recrystallized
several times from petroleum-ether. In order to quickly dissolve the
bitter substance, it should be carefully melted in a flask, and double
its volume of ether gradually added; on its cooling, we obtain beautiful
prismatic crystals, which attain a length of 1 cm., and become perfectly
pure after four or five crystallizations. The mother solutions must be
speedily evaporated if we still wish to obtain crystals; after a time
they will only furnish a resinous residue.
The hop-bitter acid melts at 92° to 93°. It is easily soluble in
alcohol, ether, benzol, chloroform, sulphide of carbon, and vinegar; to
a lesser extent in cold petroleum ether, and not at all in water.
In the analysis I obtained figures which correspond best with those
calculated from the formula C_{25}H_{35}O_{4}.
Obtained.
Calculated. ------------------------^-----------------------
-----^----- 2. Crystal. 3. Crystal. 5. Crystal. 6. Crystal.
p.c. p.c. p.c. p.c. p.c. p.c. p.c.
C 75.19 74.79 74.83 74.9 75.04 75.05 75.07
H 8.77 8.97 8.90 8.85 8.87 8.83 8.80
O 16.04
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