The Treatment of Ergot of Rye, and the Production therefrom of the Substance which Imparts to it its Valuable Properties.
Year: 1894

page_text: Date of Application, 26th Feb., 1894
Complete Specification Left, 26th Nov., 1894--Accepted, 29th Dec., 1894
PROVISIONAI. SPECIFICATION.
The Treatment of Ergot of Rye, and the Production therefrom of
the Substance which Imparts to it its Valuable Properties.
I, JAMES YATE JOHNSON of 47 Lincoln's Inn Fields in the County of
Middlesex, Gentleman do hereby declare the nature of this invention (which has
been communicated to me from abroad by C. F. Boehringer & Söhne of Waldhof
Dear Mannheim in the Empire of Germany) to be as follows:-
By maintaining certain limits of temperature and by a suitable removal of the
oil contained in ergot of rye the substance imparting to the said ergot of rye its
valuable properties can be separated or isolated in a pure condition.
This substance we have ascertained is soluble in ether acetic ether chloroform
benzol and other liquids and insoluble in petroleum ether benzin legroin petroleum
and other like liquids and these properties are according to this invention taken
advantage of to obtain the said substance in a condition of purity.
The process is performed either by first separating ergot of rye from the oil
contained therein by treatment with petroleum ether or the like and afterwards
extracting with ether the desired substance deprived of oil and freed from petroleum
ether or by directly treating ergot of rye with ether and mixing the solution thus
obtained with petroleum ether or the like always taking care that the temperature
remains below 50 degrees Centigrade.
Ether and petroleum ether are preferably employed as they boil below
50 degrees Centigrade and consequently admit of being readily removed or
separated with the employment of low temperatures. When other solvents are
employed care must be taken by the employment of a vacuum or other like means
to prevent the temperature in driving off the solvent from rising to 50 degrees
Centigrade.
Example I. 50 kilos. of pulverized ergot of rye are treated in the cold with
100 kilos. of ether and the ether is distilled off as completely as possible at the
lowest possible temperature after which petroleum ether of the boiling point of
from 36 to 42 degrees Centigrade is added until further additions cease to cause
any precipitation. By again dissolving the filtered precipitate in ether and
again precipitating with petroleum ether the substance is obtained free from oil
and in a pure condition after careful drying.
Example II. 50 kilos. of pulverized ergot of rye are first deprived of oil by
treatment with about 100 kilos. of petroleum ether of a low boiling point and
then the petroleum ether is completely removed by moderate heating after which
the remaining matter is treated with about 100 kilos. of ether. After the ether
has been distilled off at as low temperature as possible the desired substance to
be obtained remains in an almost pure condition slightly contaminated with oil.
The further purification is proceeded with in the same manner as in Example I
that is to say by further taking up in ether and precipitating with petroleum
ether. The substance can also be separated from the ether solution by means
of diluted alkalies and be separated from the salt solution by means of acids
such as sulphuric acid and also by carbonic acid. The substance obtained in
either of these ways possesses the properties of a weak acid and is in the form
of a dull yellow powder which is almost insoluble in water, benzin, ligroin,
petroleum ether, petroleum and like liquids but is soluble in acetic ether, alcohol,
chloroform, benzol, toluol and ether." In the latter the substance dissolves

page_text: readily in equal parts by weight and this property is of value in identifying and
separating it from other substances.
The substance combines with alkalies forming beautiful yellow salts which are
readily soluble in water but less readily soluble in alcohol and are insoluble in
ether. The alkaline salts are preferably obtained. by dissolving the substance in
ether and adding alcohol or soda or potash.lyes.or by introducing dry ammonia gas
in the ether solution or by causing it to flow over the dry substance.
Dated the 26th day of February 1894.
JOHNSONS & WILLCOX,
47, Lincoln's Inn Fields, London, W.C., Agents.
The Treatment of Ergot of Rye, and the Production therefrom of
the Substance which Imparts to it its Valuable Properties.
I JAMES YATE JOHNSON of 47 Lincoln's Inn Fields in the County of
London Gentleman do hereby declare the nature of this invention (which has
been communicated to me from abroad by C. F. Boehringer & Söhne of Waldhof
near Mannheim in the Empire of Germany) and in what manner the same is to
be performed to be particularly described and ascertained in and by the following
statement :-
By maintaining certain limits of temperature and by a suitable removal of the
oil contained in ergot of rye the substance imparting to the said ergot of rye its
valuable properties can be separated or isolated in a pure condition.
This substance we have ascertained is soluble in ether acetic ether chloroform
benzol and like liquids and insoluble in petroleum ether benzin ligroin petroleum
and other like liquids and these properties are according to this invention taken
advantage of to obtain the said substance in a condition of purity.
The process is performed either by first separating ergot of rye from the oil
contained therein by treatment with petroleum ether or the like and afterwards
extracting with ether the desired substance deprived of oil and freed from petroleum
ether or by directly treating ergot of rye with ether or the like and mixing the
solution thus obtained with petroleum ether or the like always taking care that the
temperature remains below 50 degrees Centigrade.
Ether and petroleum ether are preferably employed as they boil below 50 degrees
Centigrade and consequently admit of being readily removed or separated with the
employment of low temperatures. When other solvents are employed care must be
taken by the employment of a vacuum or other like means to prevent the
temperature in driving off the solvent from rising to 50 degrees Centigrade.
Example I. 50 kilos. of pulverized ergot of rye are treated in the cold with
100 kilos. of ether and the ether is distilled off as completely as possible at the
lowest possible temperature after which petroleum ether of the boiling point of
from 36 to 42 degrees Centigrade is added until further additions cease to cause
any precipitation. By again dissolving the filtered precipitate in ether and again
precipitating with petroleum ether the substance is obtained free from oil and in a
pure condition after careful drying.
Example II. 50 kilos. of pulverised ergot of rye are first deprived of oil by
treatment with about 100 kilos. of petroleum ether of a low boiling point and then
the petroleum ether is completely removed by moderate heating after which the
remaining matter is treated with about 100 kilos. of ether. After the ether has
been distilled off at as low temperature as possible the desired substance to be
obtained remains in an almost pure condition slightly contaminated with oil.
The further purification is proceeded with in the same manner as in Example I

page_text: that is to say by further taking up in ether and precipitating with petroleum ether.
The substance can also be separated from the ether solution by means of diluted
alkalies and be separated from the salt solution by means of acids such as sulphuric
acid and also by carbonic acid. The substance obtained in either of these ways
possesses the properties of a weak acid and is in the form of a dull yellow powder
which is almost insoluble in water, benzin, ligroin, petroleum ether, petroleum and
like liquids but is soluble in acetic ether, alcohol, chloroform, benzol toluol and
ether. In the latter the substance dissolves readily in equal parts by weight
and this property is of value in identifying and separating it from other substances.
Having now particularly described and ascertained the nature of the said inven-
tion and in what manner the same is to be performed I declare that what I
claim is
The treatment of ergot of rye for the production therefrom of the substance
imparting to it its valuable properties the said treatment consisting in either first
acting on the ergot of rye by means of ether or the like and afterwards depriving
the extract obtained of oil by means of petroleum-ether, or the like, in order to
isolate the substance; or first separating the oil by means of petroleum-ether or
the like and afterwards extracting by means of ether or the like and then isolating
the substance either by driving off the ether or by agitating the ether solution with
a weak alkaline solution and afterwards precipitating with acid the temperature
being always kept low all substantially as hereinbefore described.
Dated this 26th day of November 1894.
JOHNSONS & WILLCOX,
Agents.