of Artificial Musk from Hydrogenated Aromatic Hydrocarbons.
Year: 1893

page_text: Date of Application, 20th Sept., 1893
Complete Specification Left, 15th June, 1894-Accepted, 21st July, 1894
TROYDDIONAL SETNAERUATION.
Production of Artificial Musk from Hydrogenated Aromatic
Hydrocarbons.
I, ALBERT BAUR, of Mulhouse, Alsace, Doctor, do hereby declare the nature
of this invention to be as follows:-
By treating hydrometaxylene (Wallach, Annalen 259-326) with chloride of
butyle, in presence of chloride of aluminium, butylated hydrocarbon is obtained.
This, by nitration, is transformed into trinitrobutylxylene, hydrogen being
eliminated as the nitro group is introduced. This trinitro derivative is the active
musk smelling substance described in the Specifications No. 18521 of 1888,
No. 4693 of 1889 and No. 15687 of 1890.
According to my invention, I mix 108 gr. hydroxylene with 500 gr. sulphide of
carbon and 925 gr. of chloride of butyle (or the equivalent proportion of iodide or
bromide) and I add gradually about 20 gr. of chloride of aluminium. The reaction
begins at ordinary temperature and is completed by heating on the water-bath
during a few hours. The sulphide of carbon is then distilled off; water is added
to the residue and the oil is distilled with steam. The oil is separated from the
water, dried and submitted to fractional distillation. The portion distilling
between 1900 and 210° C. contains principally the butylated dihydroxylene.
50 gr. of this oil are introduced gradually into 600 to 800 gr. of a mixture.
containing one part of fuming nitric acid and two parts of fuming sulphuric acid,
containing 10 to 15 per cent. of SO, and the mixture is heated for several hours on
the water-bath, until a sample poured into water at once solidifies. All the liquid
is then poured into water and the nitro derivative which is separated out, is
crystallized from alcohol.
Dated this 20th day of September 1893.
ABEL & IMRAY,
Agents for the Applicant.
COMPLETE SPECIFICATION.
Production of Artificial Musk from Hydrogenated Aromatic
Hydrocarbons.
I, ALBERT BAUR, of Mulhouse, Alsace, Doctor, 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:-
By treating hydrometaxylene (Wallach Annalen 259-326) with chloride of
butyle in presence of chloride of aluminium, butylated hydrocarbon is obtained.
This, by nitration, is transformed into trinitrobutylxylene, hydrogen being
eliminated as the nitro group is introduced. This trinitro derivative is the active
musk smelling substance described in the Specifications No. 18521 of 1888,
No. 4693 of 1889 and No. 15687 of 1890.
According to my invention I mix 108 gr. hydroxylene with 500 gr. sulphide of
carbon and 925 gr. of chloride of butyle (or the equivalent proportion of iodide
or bromide) and I add gradually about 20 gr. of chloride of aluminium. The
reaction begins at ordinary temperature and is completed by heating on the water
bath during a few hours. The sulphide of carbon is then distilled off; water is
added to the residue and the oil is distilled with steam. The oil is separated from

page_text: the water, dried and submitted to fractional distillation. The portion distilling
between 1900 and 210° C. contains principally the butylated dihydroxylene.
50 gr. of this oil are introduced gradually into 600 to 800 gr. of a mixture
containing one part of fuming nitric acid and two parts of fuming sulphuric acid,
containing 10 to 15 per cent. of SO3, and the mixture is heated for several hours
on the water-bath, until a sample poured into water at once solidifies. All the
liquid is then poured into water and the nitro derivative which is separated out,
is crystallized from alcohol.
Having now particularly described and ascertained the nature of this inven-
tion and in what manner the same is to be performed, I declare that what I
claim is :-
The production of artificial musk by nitrating butylated hydrocarbon and
treating the product substantially as described.
Dated this 15th day of June 1894.
ABEL & IMRAY,
Agents for the Applicant.