IMPROVEMENTS IN THE MANUFACTURE OF ARTIFICIAL ALKALOIDS DERIVED FROM COAL TAR, AND IN THE PREPARATION OF SALTS OF THE SAID ALKALOIDS
Year: 1870

page_text: LETTERS PATENT to John Casthelaz, of Number Nineteen, Rue
Sainte Croix de la Bretonnerie, in the City of Paris, Merchant, for
the Invention of "IMPROVEMENTS IN THE MANUFACTURE OF ARTIFICIAL
ALKALOIDS DERIVED FROM COAL TAR, AND IN THE PREPARATION OF SALTS OF
THE SAID ALKALOIDS."
.Sealed the 25th October 1870, and dated the 18th May 1870.
PROVISIONAL SPECIFICATION left by the said John Casthelaz at the
Office of the Commissioners of Patents, with his Petition, on the
18th May 1870.
I, JOHN CASTHELAZ, of Number Nineteen, Rue Sainte Croix de la
Bretonnerie, in the City of Paris, Merchant, do hereby declare the
nature of the said Invention for "IMPROVEMENTS IN THE MANUFACTURE OF
ARTIFICIAL ALKALOIDS DERIVED FROM COAL TAR, AND IN THE PREPARATION OF SALTS
OF THE SAID ÅLKALOIDS," to be as follows:-
:―
My Invention' relates in the first place to the extraction of analine
toluidine, naphtylamine, or other artificiál alkaloid from the crude
product or crude paste in which it is contained, and for this purpose I.

page_text: employ a liquid hydrocarbon instead of the usual mode of extraction by
means of steam or distillation on fire..
Any liquid hydrocarbon which evaporates at a low temperature
without leaving a residue may be employed, but I prefer to use a
petroleum spirit evaporable at a low temperature. The said crude paste
is to be heated and mixed with the liquid hydrocarbon which dissolves
the alkaloid. The solution of the alkaloid in the hydrocarbon collects
on the surface of the paste, and is to be drawn off and rectified. This
method of extraction is particularly suitable to the preparation of
naphtylamine.
A further portion of my Invention relates to the preparation of pure
chlorhydrates of analine, toluidine, naphtylamine, and other artificial
alkaloids of a regular and invariable quality, or composition, white,
entirely neutral, and soluble in water. It is of advantage that a good
commercial chlorhydrate.should possess all the above-named qualities,
and such a salt of analine is especially required for the production of a
good analine black. The chlorhydrates are usually obtained by mixing
analine, toluidine, naphtylamine, or other artificial alkaloid, with liquid
hydrochloric acid, the mixture being concentrated by evaporation until
the salt is obtained. The salt so obtained either in crystals or in cakes
is not neutral, it does not readily or entirely dissolve in water, it is more
or less colored, it contains more or less water according to the degree of
desiccation, and it is liable to deterioration or alteration in composition.
When producing the aforesaid chlorhydrates in manner according
with my Invention, I dissolve the artificial alkaloid, such as analine,
toluidine, or naphtylamine in a liquid hydrocarbon, and I pass into the
solution so formed a sufficient quantity of dry hydrochloric gas until
all the chlorhydrate is precipitated. When the chemical action ceases
the resultant salt deposited at the bottom of the vessel is collected, and
in order the more rapidly to discharge therefrom the liquid held in
suspension the said salt is or may be partly dried by means of an hydro-
extractor, the drying being afterwards completed in a stove or drying
room. The resultant of the above described process is an anhydrous
neutral salt, regular and unvarying in composition and strength, colorless,
and pulverulent.
Any liquid hydrocarbon which evaporates at a low temperature
without leaving a residue may be used for the solution of the alkaloid.
I prefer a petroleum spirit distilling or evaporating at a low temperature.

page_text: By treating the solution of the aforesaid artificial alkaloids in a liquid
hydrocarbon with bromhydric, iodhydric, sulphurous acid or other
SPECIFICATION in pursuance of the conditions of the Letters Patent,
filed by the said John Casthelaz in the Great Scal Patent Office
on the 12th November 1870.
TO ALL TO WHOM THESE PRESENTS SHALL COME, I, JOHN
CASTHELAZ, of Number Nineteen, Rue Sainte Croix de la Brettonerie,.
in the City of Paris, Merchant, send greeting.
WHEREAS Her most Excellent Majesty Queen Victoria, by Her
Letters Patent, bearing date the Eighteenth day of May, in the year of
our Lord One thousand eight hundred and seventy, in the thirty-fourth
year of Her reign, did, for Herself, Her heirs and successors, give and
grant unto me, the said John Casthelaz, Her special license that I, the
said John Casthelaz, my executors, administrators, and assigns, or such
others as I, the said John Casthelaz, my executors, administrators, and
assigns, should at any time agree with, and no others, from time to time
and at all times thereafter during the term therein expressed, should
and lawfully might make, use, exercise, and vend, within the United
Kingdom of Great Britain and Ireland, the Channel Islands, and Isle of
Man, an Invention for IMPROVEMENTS IN THE MANUFACTURE OF ARTIFICIAL
ALKALOIDS DERIVED FROM COAL TAR, AND IN THE PREPARATION OF SALTS OF THE
SAID ALKALOIDS," upon the condition, amongst others, that I, the said
John Casthelaz, by an instrument in writing under my hand and
seal, should particularly describe and ascertain the nature of the said
Invention, and in what manner the same is to be performed, and
cause the same to be filed in. the Great Seal Patent Office within 'six
calendar months next and immediately after the date of the said Letters
Patent.
66
NOW KNOW YE, that I, the said John Casthelaz, do hereby declare
the nature of the said Invention, and in what manner the same is to be
performed, to be particularly described and ascertained in and by the
following statement, that is to say :—
My Invention relates in the first place to the extraction of aniline,
toluidine, naphtylamine, or other artificial alkaloids, from the crude

page_text: product or crude paste in which it is or they are contained, and for this
purpose I employ a liquid hydrocarbon instead of the usual mode of
extraction by means of steam or distillation on fire.
Any liquid hydrocarbon which evaporates at a low temperature
without leaving a residue may be employed, but I prefer to use a 5
petroleum spirit evaporable at a low temperature. The said crude paste
is to be heated by steam and mixed with the liquid hydrocarbon which
dissolves the artificial alkaloid, this mixture being stirred up. The
solution of the artificial alkaloid in the hydrocarbon collects on the
surface of the paste and is to be drawn off and rectified. This 1
operation is to be repeated two or three times or as often as may be
required until the artificial alkaloid is completely extracted. This
method of extraction is particularly suitable to the preparation of
naphtylamine.
A further portion of my Invention relates to the preparation of pure 1
chlorhydrates of aniline, toluidine, naphtylamine, and other artificial
alkaloids of a regular and invariable quality or composition, white,
entirely neutral, and entirely soluble in water. It is of advantage that a
good commercial chlorhydrate should possess all the 'above-named
qualities, and such a salt of aniline is especially required for the pro-
duction of a good aniline black. The chlorhydrates are usually obtained
by mixing aniline, toluidine, naphtylamine, or other artificial alkaloids,
with liquid hydrochloric acid, the mixture being concentrated by
evaporation, until the salt is obtained. The salt so obtained, either in
crystals or in cakes, is not neutral; it does not entirely dissolve in water;
it is more or less coloured; it contains more or less water, according to
the degree of dessication, and it is liable to deterioration or alteration in
composition.
When producing the aforesaid chlorhydrates in manner according
with my Invention, I dissolve one part of the artificial alkaloid, such as
aniline, toluidine, or naphtylamine in fifteen parts of a liquid hydro-
carbon, and I pass into the solution so formed a sufficient quantity of
dry hydrochloric acid gas, until all the artificial alkaloid is saturated
by the hydrochloric acid gas. When the chemical action ceases the
resultant salt, hydrochlorate of aniline, toluidine, or naphtylamine
deposited at the bottom of the vessel is collected, and in order the
more rapidly to discharge therefrom the liquid held in suspension,
the said salt is or may be partly dried by means of a hydro-extractor,

page_text: the drying being afterwards completed in a stove or drying room.
The resultant of the above described process is an anhydrous neutral
salt, regular and unvarying in composition and strength, colorless and
pulverulent.
Any liquid hydrocarbon which evaporates at a low temperature
without leaving a residue may be used for the solution of the artificial
alkaloid. By treating the solution of the aforesaid artificial alkaloids in
a liquid hydrocarbon with bromhydric acid, iodhydric acid, sulphurous
acid, or other volatile or gaseous acid, other salts may be obtained.
Having now described the nature of my Invention, and means for
carrying the same into practical effect, I would have it to be understood
that I claim the employment of liquid hydrocarbons in the preparation
of artificial alkaloids derived from coal tar, and I further claim the
preparation of pure hydrochlorates of aniline, toluidine, naphtylamine,
by passing dry hydrochloric acid gas into a liquid hydrocarbon
containing one of the said artificial alkaloids in solution.
In witness whereof, I, the said John Casthelaz, have hereunto set
my hand and seal, this Eleventh day of November, in the year.
of our Lord One thousand eight hundred and seventy..
AD