The Manufacture of Pharmaceutical Compounds.
Year: 1896

page_text: Date of Application, 26th May, 1896
Complete Specification Left, 23rd Feb., 1897-Accepted, 17th Apr., 1897
IRUVIDIONAL DIBUIFICATIVA.
[Communicated from abroad by THE FARBENFABRIKEN, vormals FRIEDRICH
BAYER & Co., of Elberfeld, Germany.]
The Manufacture of Pharmaceutical Compounds.
I HENRY EDWARD NEWTON of The Office for Patents, 6 Bream's Buildings,
Chancery Lane in the County of London, Patent Agent, do hereby declare the
nature of this invention to be as follows:-
My foreign correspondents described in the Application 12295 a process for
the production of the so-called active substance of thyroid glands, which process
consists in heating the said glands with dilute acids, and they found some time
afterwards that dilute alkalies might be used in this process, instead of dilute acids,
with the same result.
On applying, now, the said process to spongiæ, laminariæ, fucus, and the like
bodies, containing, as is well known, iodine compounds, my foreign correspondents
have found that these iodine compounds are readily isolated in pure form by the
said process, and they have also found that the iodine compounds thus obtained
show a physiological effect very similar to that produced by the active substance of
thyroidea, and therefore may be used instead of this preparation for medical
purposes.
My foreign correspondents illustrate their process of isolating the iodine
compounds contained in sponges, by the following example, the parts being by
weight:-
EXAMPLE.
5 parts of common sponge are heated together with about from 20 to 30 parts
of dilute sulphuric acid (containing about 5 per cent. H₂SO) at 100 degrees
Centigrade, during about from 15 to 30 hours, the result being that the sponge
slowly falls into small pieces, a considerable quantity of sand separating therefrom.
The liquid thus obtained is allowed to cool; then it is filtered off, and the residue
is mixed with caustic soda-lye (containing about from 1 to 2 per cent. NaOH).
Thus the iodine compounds contained in the residue are dissolved. The liquid is
filtered off from the undissolved parts, and the iodine compounds are precipitated
therefrom by means of dilute acids, in the form of a dark red-brown precipitate,
which is filtered off, washed with water, and dried. The iodine compound thus
isolated forms an almost black powder, which is insoluble in water, almost insoluble
in alcohol, but readily soluble in alkalies, and which, as above mentioned, produces
a physiological effect similar to that of the active substance of thyroidea.
My foreign correspondents do not limit themselves to the particulars given in
the above example, as these may be varied. For instance, more
or less
concentrated sulphuric acid may be employed instead of 5 per cent. sulphuric acid,
or other mineral acids may be used instead of sulphuric acid; likewise the
concentration of the caustic soda-lye employed in the process may be varied, or
other alkalies may be used instead of soda.
As above mentioned, the hereinbefore described process of isolating the active
iodine compounds contained in sponges and the like, may also be carried out in
Price8d

page_text: heating the said bodies with dilute alkalies instead of dilute acids. In this case,
a solution is obtained containing the iodine compounds, which are precipitated
therefrom by acidulating the solution.
The hereinbefore defined process applies not only to sponges, but the active
iodine compounds contained in laminaria, fucus, and all the like bodies, may also
be isolated in the same manner.
NEWTON & SON,
Agents for the Applicant.
The Manufacture of Pharmaceutical Compounds.
I HENRY EDWARD NEWTON of The Office for Patents, 6 Bream's Buildings,
Chancery Lane, in the County of London, Patent Agent, 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 :-
My foreign correspondents described in the Specification of Letters Patent
No. 12295, dated 25th June 1895, a process for the production of the so-called
active constituent of thyroid glands, which process consists in heating the said
glands with dilute acids. They subsequently found that dilute alkalies can be used
in this process, instead of dilute acids.
On now, applying the said process to spongiæ, laminaria, fucus, and the like
materials, containing iodine compounds, my foreign correspondents have found
that such iodine compounds are readily separated by the said process, and they
have also found that the physiological action of the iodine compounds so obtained,
is very similar to that of the active substance of thyroidea (thyroid glands),
and therefore may be used, instead of this preparation, for medical purposes.
My foreign correspondents are aware of the publication of Hundeshagen
(Zeitschrift für angewandte Chemie, 1895, p. 474), who bas already treated sponge
with,acids and alkalies, but this author did not obtain the active iodine compound
separated by the new process of my foreign correspondents, as he heated the
sponge with acids until it dissolved and underwent decomposition, hydrogen
iodide and other gaseous iodine compounds being evolved. By dissolving sponge
in hot alkalies, neutralizing and evaporating the solution, extracting the residue
with alcohol, and evaporating this alcoholic solution, Hundeshagen, it is true,
obtained an "amorphous syrup-like" compound containing iodine, but the
substance produced by the process now described is different from the compound
obtained by Hundeshagen, as it is almost insoluble in alcohol and in alcoholic
soda-lye.
My foreign correspondents illustrate their process of isolating the iodine
compounds contained in sponge by the following example, the parts being by
weight.
EXAMPLE.
5 parts of common sponge are heated together with about 20 to 30 parts of
dilute sulphuric acid (containing about 5 per cent. H₂SO), at 100 degrees
Centigrade, during about 15 to 30 hours, the result being, that the sponge slowly
falls to pieces, a considerable quantity of sand separating. The liquid thus
obtained is filtered when cold, and the residue is mixed with caustic soda lye
(containing about 1 to 2 per cent. NaOH), to dissolve the iodine compounds
present in the residue. The liquid is filtered from the andissolved matter, and

page_text: the iodine compounds are precipitated from the filtrate by dilute acids in the form
of a dark red-brown precipitate, which is filtered off, washed with water, and
dried.
The insoluble residue obtained by heating the sponge with acids can also be
purified by treating it with hot alcohol, which dissolves the impurities, whilst the
pure active substance remains undissolved.
The iodine compound thus isolated and purified, forms an almost black powder,
insoluble in water, almost insoluble in alcohol or in alcoholic soda lye, but readily
soluble in alkali lye. As above mentioned, its physiological action is similar to
that of the active constituent of thyroidea.
My foreign correspondents do not limit themselves to the particulars given in
the above example, as these may be varied. For instance, more or less
concentrated sulphuric acid may be used, instead of 5 per cent. sulphuric acid, or
other mineral acids may be used instead of sulphuric acid; likewise, the
concentration of the caustic soda-lye employed in the process may be varied, or
other alkalies may be used instead of soda.
. As above mentioned, the isolation of the active iodine compounds contained in
sponge may be carried out by heating them with dilute alkalies, instead of using
dilute acids. In this case, solutions are obtained containing the iodine compounds,
which are precipitated therefrom by acids.
The hereinbefore defined processes apply not only to spongiæ, but also to
laminariæ, fucus, and the like materials.
Having now particularly described and ascertained the nature of the said inven-
tion and in what manner the same is to be performed (as communicated to me from
abroad), I declare that what I claim is :-
1. The process for obtaining the active iodine compounds from spongiæ,
laminariæ, fucus, and the like materials, which process consists in treating these
materials with dilute acids, and filtering off the insoluble residues.
2. The process for obtaining the active iodine compounds from the materials
defined in the preceding Claim 1, by treating these materials with dilute alkalies,
filtering the solution from the insoluble residue, and separating the active substance
by the addition of acids to the alkaline filtrate.
3. The process for purifying the active substances obtained in the manner
defined in the foregoing Claims 1 and 2, either by dissolving the substances in
dilute alkalies, filtering, and subsequently precipitating the active substances by
the addition of acids to the filtrate, or by treating those substances with hot alcohol,
to dissolve out impurities.
4. As new articles of manufacture:-The new iodine compounds obtained in the
manner claimed in the foregoing claims, or in any other manner yielding the same
result.
5. The use of the hereinbefore defined new iodine substances for medical
purposes.
Dated thie 23rd day of February 1897.
NEWTON & SON,
Agents for the Applicant.