Improvements in and connected with the Manufacture of Oxy- quinoline-phenolsulphonic-oxyquinoline and its Homologues.
Year: 1892

page_text: Date of Application, 1st Dec., 1892-Accepted, 7th Jan., 1893
COMPLETE SPECIFICATION.
Improvements in and connected with the Manufacture of Oxy-
quinoline-phenolsulphonic-oxyquinoline and its Homologues.
We, ADOLF LEMBACH of Biebrich a Rhein, Manufacturer, and CARL JOSEF
WOLFF, of Wiesbaden, Manufacturer, both in the German Empire, do hereby
declare the nature of this invention, and in what manner the same is to be
performed, to be particularly described and ascertained in and by the following
statement:-
This invention relates to the manufacture of oxyquinoline-phenolsulphonic-
oxyquinoline and its homologues, the product manufactured being capable of
utilisation as an intermediate in the production of colouring matters.
In carrying out our invention we may heat together phenolsulphonic-oxyquinoline
or its homologues with oxyquinoline or its homologues in molecular proportions
until their chemical combination takes place; or, we may heat together phenol,
oxyquinoline, and sulphuric acid in the proportions of one molecule of phenol, two
molecules of oxyquinoline, and one molecule of sulphuric acid; or, finally, we may
employ one molecule of phenolsulphonic acid with two molecules of oxyquinoline
or its homologues with the addition of three molecules of water at 100 degrees C.
We prefer to proceed according to either of the following processes :-
(1) 194 parts of freshly prepared phenolsulphonic acid (prepared from 94 parts
of phenol and 100 parts of sulphuric acid) are mixed with 290 parts of o-oxyquino-
line which has previously been dissolved by boiling with 54 parts of water. The
chemical combination takes place immediately. During cooling, the product
solidifies to a firm crystalline mass which may be ground to powder.
(2) 94 parts of phenol (one molecule); 290 parts (two molecules) of oxyquinoline;
and 54 parts (three molecules) of water are dissolved together on a water bath.
With an increase of temperature the mixture turns yellow. It is then cooled down
to 80 degrees C., and a mixture of 100 parts of chemically pure sulphuric acid, and
100 parts of water is added in a gentle stream so that the contents of the vessel do
not exceed a temperature of 100 degrees C. The mixture is then allowed to cool
with constant stirring, and the resulting crystals are separated from the water by
draining or other suitable means.
The product obtained as hereinbefore described may be readily re-crystallised
from its aqueous solution, producing well formed amber-yellow transparent hexagonal
columns which may be dissolved in water in any proportions and which contain
four molecules of H₂O. The crystals melt at from 78 to 83 degrees C.
2>
The empirical formula of the product is CHS, N2,010, and its molecular weight
is 536-08 as shewn by the following analysis by Privy-Aulic-Councillor Professor
Found
Calculated
Carbon
53.90
53-723
Hydrogen
5.25
5.223
Nitrogen
5.37
5-238
Sulphur
6.02
5.969
Oxygen
29.46
29.847

page_text: распоютрибите ни,
4 molecules of water.
Having now particularly described and ascertained the nature of our said inven- 5
tion and in what manner the same is to be performed, we declare that what we
claim is :-
1. The manufacture or production of oxyquinoline-phenolsulphonic-oxyquinoline
and its homologues substantially as and by the means hereinbefore described.
2. As a new article of manufacture, oxyquinoline-phenolsulphonic oxyquinoline 1
and its homologues, prepared or manufactured substantially as hereinbefore
described.
WILLIAM E. HEYS,
Agent for the Applicants.