Year: 1889

page_text: Date of Application, 27th Apr., 1889
Complete Specification Left, 22nd Jan., 1890-Accepted, 19th Apr., 1990
Z2 (3/23/2
TO/2 T2 U.
This methylmercaptol, forming a clear colourless oily liquid, is separated from the
water formed along with it in this reaction and the surplus of acid is washed out.
For a further purification the mercaptol can be distilled by incans of steam, it has less
specific gravity than water and smells less strong and disagreeable. It proves to be
very volatile.
As a means of condensation instead of gaseous hydrochloric acid, an aqueous
solution of hydrochloric or sulphuric acid can be employed, but in any case it is
necessary to keep the temperature very low, to avoid loss.
This methylmercaptol is transformed into the corresponding disulphonate by
oxydation with permanganate of potassium according to the following formula
(CH), C (SCH3)2 +40= (CH2)2 C (SO₂ CH3)2.
This tetramethyldisulphon methane is brought by us on the market under the name
of methylsulphonal, it is soluble in water and crystallizes in large rhombic leaves.
Its melting point was found to be between 119-120° Centigrade uncorrected
atmospheric pressure.
Dated this 27th day of Anril 1880

page_text: CUM LELE SPECIFICATION.
The Manufacture of an Improved Medical Compound.
I, WILLIAM ROBERT LAKE, of the firm of Haseltine, Lake & Co., Patent Agents,
Southampton Buildings, in the County of Middlesex 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 an improved medical compound.
Baumann has described in the Reports of the German Chemical Society 1885
page 884 "Berichte der Deutschen Chemischen Gesellschaft" a few mercaptols of
inost specific properties.
I have discovered a new mercaptol which is essentially different from any at present
known.
It is produced in the following manner 96 kilogrammes of methylmercaptan
obtained in the well known manner are mixed with 5-8 kilogrammes of acetone and
the mixture well cooled, under constant cooling gaseous hydrochloric acid is introduced
when a reaction takes place, through which methylmercaptol is formed after the
formula:
(CH, SH), + (CH,), CO=(CH,), C (SCHs), + H, O.
This reaction is accompanied by a certain loss, if the methylmercaptan is not brought
into reaction after being dissolved in a suitable solvent which at the same time is
indifferent towards the other ingredients, I therefore first dissolve the methyl-
mercaptan in suitable solvents such as alcohol, benzol, toluol, methylalcohol, other,
bromethyl and then allow the above described reaction to take place.
Instead of the above named solvents their homologues may be employed with
similar results.
After the reaction is completed, the water formed by the reaction is first separated
and after this the solvent is driven off and the methylmercaptol remains, this represents
a clear colourless oily liquid very refractive not soluble in water, easily soluble in
alcohols, ethers, chloroform, chlorethyl iodide of methyl and the like. If in a pure
state, it can be distilled without decomposition and its boiling point is at 168-170° C.
uncorrected.
It is of less specific gravity than water and smells less strong and disagreeable than
the aethylmercaptol.
As a means of condensation instead of gaseous hydrochloric acid an aqueous
solution of hydrochloric or sulphuric acid can be employed, but in any case it is
necessary to keep the temperature very low, to avoid loss.
This methylmercaptol is transformed into the corresponding disulphone by oxidation
with permanganate of potassium according to the following formula
(CH), C (SCH)2 + 40 (CH3), C (SO, CH3)2.
This tetramethyldisulphon methane I call by the name of "methylsulphonal," or
"methonal," it is soluble in water and cristallizes in large rhombic leaves. Its melting
point was found to be between 119-120° Centigrade uncorrected atmospheric pressure.
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 by
my foreign correspondent I declare that what 1 claim is :-
The production of tetramethylmercaptol and the transformation of such into its
disulphone by means of oxidation substantially as described.
Dated this 22nd day of January 1890
HASELTINE, LAKE & Co.,
45, Southampton Buildings, London, Agents for the Applicant.