IM- PROVEMENTS IN THE MANUFACTURE OF QUININE
Year: 1846

page_text: TO ALL TO WHOM THESE PRESENTS SHALL COME, I, JOHN
LLOYD BULLOCK, of Conduit Street, Hanover Square, Chemist, send greeting.
WHEREAS Пe present most Excellent Majesty Queen Victoria, by Her
Royal Letters Patent under the Great Seal of the United Kingdom of Great
Butain and Ireland, bearing date at Westminster, the Twelfth day of May,
in the ninth year of Her reign, did, for Herself, Her heirs and successors,
give and grant unto me, the said John Lloyd Bullock, my exors, aduiors,
and assigns, Iler especial licence, full power, sole privilege and authority,
that I, the said John Lloyd Bullock, my exors, adñiors, and assigns,
or such others as I, the said John Lloyd Bullock, my exors, admors,
or assigns, should at any time agree with, and no others, from time
to time and at all times during the term of years therein expressed,
should and lawfully might make, use, exercise, and vend, within England,
Wales, and the Town of Berwick-upon-Tweed, my Invention of "IM-
PROVEMENTS IN THE MANUFACTURE OF QUININE," being a communication; in
which said Letters Patent is contained a proviso that I, the said John
Lloyd Bullock, shall cause a particular description of the nature of my said
Invention, and in what manner the same is to be performed, by an instrument
in writing under my hand and seal, to be inrolled in Her said Majesty's High
Court of Chancery within six calendar months next and immediately after
the date of the said in part recited Letters Patent, as in and by the same,
reference being thereunto had, will more fully and at large appear.

page_text: NOW KNOW YE, that in compliance with the said proviso, I, the said
John Lloyd Bullock, do hereby declare that the nature of my said Invention,
and the manner in which the same is to be performed, are fully described
and ascertained in and by the following statement thereof, that is to say.—
In the preparation of quinine, sulphate of quinine, or other saline com-
pounds, after the separation of the crystalline sulphate or other salt, there
remains a dark colored mother liquor, which, being treated by the manu-
facturer with an alcalı or alcaline carbonate, yields a precipitate which in
drying agglutinates into a resinous-like mass, called by the manufacturer
chinoidine o quinoidine, which is regarded as of little value. Sometimes the
said mother liquor is simply evaporated, the residue is then a mixture of
NOW KNOW YE, that in compliance with the said proviso, I, the said
John Lloyd Bullock, do hereby declare that the nature of my said Invention,
and the manner in which the same is to be performed, are fully described
and ascertained in and by the following statement thereof, that is to say.
In the preparation of quinine, sulphate of quinine, or other saline com-
pounds, after the separation of the crystalline sulphate or other salt, there
remains a dark colored mother liquor, which, being treated by the manu-
facturer with an alcalı or alcaline carbonate, yields a precipitate which in
drying agglutinates into a resinous-like mass, called by the manufacturer
chinoidine oi quinoidine, which is regarded as of little value. Sometimes the
said mother liquor is simply evaporated, the residue is then a mixture of
chinoidine with an acid
My discovery includes,―
First, the preparation of either of these products in a purified state, so as to
enable me to reduce it to a powder, which I call purified chinoidine, and the
forming of a solution of this in alcohol or other vehicle and certain saline
compounds.
Second, the separation of amorphous quinine, and reducing it to powder,
from the chinoidine or purified chinoidine. by means of a solution in ether;
and also the forming solutions of amorphous quinine in alcohol or other vehicle,
and saline compounds.
Third, the substance left after digesting in ether, which, having basic
properties, I call basic extract of bark, a solution of the same in alcohol or
other vehicle, and saline compounds of the same.
Fust, Preparation of Punified Quinoidine or Chinoidine.-I take three
pounds of the residue of quinine manufacture termed chinoidine (which should
be soluble in alcohol and in dilute sulphuric acid, and insoluble in water), nine
ounces by measure of concentrated sulphuric acid, diluted with one gallon of
water, and dissolving the chinoidine therein, I then pass sulphuretted by diogen
through the solution of nine hours, for the purpose of precipitating metallic
matters and other impurities. The mixture is then to be filtered through
paper or other suitable material, as is well understood by chemists. It is then
boiled to drive off excess of sulphuretted hydrogen, and an alcalı or alcaline
carbonate added to precipitate the chinoidine. I use commonly for the above-
named quantity three pounds of carbonate of soda, dissolved in one gallon of
distilled water. The precipitate obtained is then to be well washed with
distilled water, and dried over a water bath. Towards the conclusion of the
drying, and in order to dry it more effectually, I place it in a chloride of
calcium bath, and heat it a few degrees higher than 212° It is then reduced

page_text: to powder, and kept in well closed bottles. This punified chinoidine may also
be kept in solution in alcohol or other velucle, or made into saline compounds
I prefer to sell it in a state of powder, it being more convenient in that form.
T also prepare various saline compounds of purified chinoidine by taking at
the rate of one twelfth less than of the amorphous quinine hereafter explained,
and mix it with acids, as hei cafter explained in respect to amorphous quinine.
In some cases it is desirable to dissolve the purified chinoidine in alcohol
before mixing with the acids. These saline compounds I prepare for sale
either in solution, or by evaporating them to the solid state, and reduce them,
when they will allow of it, to powder. In all cases the preparation should be
kopt in well-closed bottles
The Preparation of Amorphous Quinine.-I take three pounds of chinoidine,
as before, or in the punified state, as above described (for this purpose it is
best to use it before it is fully dried), and mix it well with twice its weight of
pure sand, and digest it in nine pints of ether (commonly known as sulphuric
ether), the specific gravity of the ether I believe most suitable being about
735 I stu up the mixture thice or four times during the digestion, which
should continue twelve hours, and pour off the solution. To the residue I add
nine pints of fiesh ether, and proceed as before. I mix the two solutions, and
allow them to settle. When perfectly bight, I pour off the fluid from the
sediment into a retort or suitable vessel, and distill off the ether by means of
a water bath The substance left in the vessel is to be dried in the same
manner as is directed for the punified chinoidine To this residue I apply the
term amorphous quinine. The saline compounds are prepared by taking one
equivalent of an acid in solution, and dissolving in it an equivalent of the
amorphous quinine. Considering carbon 6, oxygen 8, hydiogen 1, I take one
hundied and sixty two parts of amorphous quinine to each equivalent of acid,
all which is well understood by chemists, and I form basic, neutral, or acid
salts, in the usual way.
Basic Extract of Bark -The residue left upon treating chinoidine with
ether in order to extract the amorphous quinine contains also valuable
medicinal matter. I take any given amount of this product, and calculating
the amount of dry substance it contains, treat it with six times its weight of
alcohol, generally prefening it 56° overproof I decant the clear fluid, and
evaporate it to dryness in the same manner as with amorphous quinine
this product I apply the designation basic extract of bark. Or I prepare this
as follows-To three pounds of the dry residue as above I add nine ounces by
measure of concentrated sulphuric acid, diluted with one gallon of water, and
dissolve the same, and through this solution I pass sulphuretted hydrogen, and
To

page_text: proceed in the same manner as when producing purified chinoidine, and in
making solutions and saline compounds therefrom.
Having thus described the nature of the Invention, and the manner in which
the same is to be performed, I would have it understood that I do not confine
myself to the details herein described, so long as the peculiar character of
either part of the Invention be retained; but what I claim is,-First, the
manufacture of what I have called "purified chinoidine," by purifying and
reducing that matter to a state of powder, as herein described. And I also
claim the making alcoholic and other solutions of such purified chinoidine, and
also the producing saline compounds thereof.
Secondly, I claim the manufacture of what I have called "amorphous
quinine," by parating the matter soluble in ether from other matters, as heicin
described. I also claim the preparing alcoholic, ethereal, and other solutions
thereof And I also claim the preparation of salino compounds of the same.
And, thirdly, I claim the manufacture of what I have called "the basic
extract of bark," by separating such product by ether from the soluble matter,
and preparing such extract as herein descubed, and producing alcoholic and
other solutions and saline compounds thereof.
In witness whereof, I, the said John Lloyd Bullock, have hereunto sct
my hand and scal, this Twelfth day of November, in the year of our
Loid One thousand eight hundied and forty-six.