The Manufacture of a Substitute for Musk.
Year: 1888

page_text: Date of Application, 18th Dec., 1888
Complete Specification Left, 18th Sept.. 1889-Accepted 26th Oct
1889
PROVISIONAL SPECIFICATION.
The Manufacture of a Substitute for Musk.
We, EMIL SCHNAUFER, Chemist, and HEINRICH HUPFELD, Chemist, both of
Frankfort on the Main, Germany, do hereby declare the nature of this invention to
be as follows:-
This Invention relates to the manufacture of a substitute for musk. To produce
this artificial substitute; heat three kilogrammes of metaxylol with two kilogrammes
of Isobutylalcohol and nine kilogrammes of chloride of zinc in a digester to from 220°
to 240° until the pressure which at the commencement is from twenty-five to twenty-
nine atmospheres sinks to below six atmospheres. The duration of the operation is
from five to eight-days. The resulting hydrocarbon, corresponding to the
formula C, H, is collected and the fraction which distils over at from 190° to 230°
is nitrated with H NO, or with H NO, and H, SO, whilst being cooled.
The
product of the reaction is poured into water, whereupon a reddish brown oil separates
out which is washed several times with alkaline water. The formula of this oil
is C₁s H1, NO, and in a concentrated condition it possesses a sweet smell whilst in a
dilute solution it gives off a penetrating and enduring musk-like odor.
Dated this 18th day of December 1888
COMPLETE-SPECIFICATION.
The Manufacture of a Substitute for Musk.
We EMIL SCHNAUFER, Chemist, and HEINRICH HUPFELD, Chemist, both of
Frankfort on the Main, Germany, do hereby declare the nature of this inven-
tion 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 a substitute for musk.
Aromatic hydrocarbons containing the iso-propyl, Iso-butyl or Iso-amyl group (as a
side group) on treatment with fuming nitric acid or a mixture of strong nitric acid
(40° to 44° B.) and sulphuric acid (66° B.) produce derivatives which, in very dilate
alcoholic solution furnish a liquid possessing an odour resembling tincture of musk in
the highest degree.
In the Provisional Specification only one example of the process is given by way
of illustration, but of course the process may be carried out with the other well known
homologues.
The hydrocarbons may be produced in the ordinary way, but we produce them by
the following operation.
Toluol or Xylol is heated in a digester with Iso-propyl-or Iso-butyl-or Iso-amyl-
alcohol in molecular quantities with the addition of, from 4 to 5 times the quantity of
chloride of zinc to the boiling point of the hydrocarbon, or to about 40° or 50° above
the boiling point of alcohol, until the pressure-which at the commencement was equal
to about twenty six atmospheres, sinks to a little above two or three atmospheres.
The product of the reaction is subjected to fractional distillation.
By the above process the following hydrocarbons are obtained :-
1. From Toluol, Methylisopropyl-benzole.

page_text: 2. From Xylol, Dimethylisopropyl-benzole.
Dimethylisobutyl-benzole.
Dimethylisoamyl-benzole.
To produce the musk substitute we add to the above mentioned hydrocarbons, which
during the operation should be kept thoroughly cool, a little more than the molecular
quantity of fuming nitric acid or nitro-sulphuric acid. The acid should be gradually
run in and the whole is then allowed to stand 'undisturbed for from one to two hours,
the resulting mass being then poured into water in order to get rid of the excess of
acid. The well washed substances thus obtained are then subjected to distillation by
means of steam whereupon simultaneously formed bodies which smell like nitro-benzol
and overpower the musk odour readily distil over, whilst the pure substances remain
behind.
Having now particularly described and ascertained the nature of the said inven-
tion and in what manner the same is to be performed, we declare that what we
*claim is :-
The production of the herein described substances (having in alcoholic solution a
musk like odour) from the afore-mentioned hydrocarbons by means of nitric acid or
nitro-sulphuric acid substantially as specified.
553
E. SCHNAUFER.
H. HUPFELD.
By A. M. & Wm. Clark,
53, Chancery Lane, London, Patent Agents.