Year: 1896

page_text: Date of Application, 3rd Nov., 189
Complete Inonification Lafe 10th
1007
in
A
1007
I, ADOLF BLAILE, of 24, Hafnerstrasse, Zürich, in the Republic of Switzerland,
Manufacturer, do hereby declare the nature of this invention to be as follows:-
This invention has for its object an improved process for the manufacture of
artificial musk..
This process is carried out as follows:-
100 parts by weight of terpinol are mixed with 100 parts of rutyl-alcohol so that
a clear solution of both substances results. The 200 parts of solution obtained are
poured into 100 parts by weight of sulphuric acid of 66° Beaumé with constant
stirring and cooling of the latter, and after the completion of the pouring in, the
mixture is vigorously stirred for 6 hours further.
The sulphuric acid compound obtained by the above operations is gradually
poured into a quantity of 1000 parts by weight of concentrated nitric acid free
from chlorine, the necessary care being observed. It is necessary for this that the
sulphuric acid should be maintained in constant movement by stirring and the
temperature for the nitric acid should not exceed 8° Celsius. After these
operations have been terminated, the mixture is warmed for about 4 hours to
70° (or about 70°) Celsius and then cooled down and poured into 20,000 parts by
weight of water, which is vigorously stirred during the admixture. It forms then
an amorphous clear brown deposit, which is obtained by filtration.
The clear brown deposit obtained is pressed, dried and preferably made into
the form of cakes and constitutes the new perfume in a crude condition. For
the purpose of obtaining the perfume pure, the brown cakes obtained in the
manner hereinbefore described are ground to a fine powder and treated with
hot water until a sample of the brown mud dissolved with alcohol shows a neutral
reaction.
This last mentioned substance (mud) is filtered and dried and repeatedly purified
by means of suitable solvents, such, for instance, as petroleum-ether, until a clear
yellow crystalline substance is obtained. This latter has a tender, agreeable musk
scent and is used in perfumery.
It must also be mentioned that by the process hereinbefore described a musk-
smelling crystalline substance is obtained, if instead of the terpinol mentioned at
the commencement of this specification an equal quantity by weight of turpentine
oil or eucalyptus or another body be employed which shows the chemical-character
of the so-called terpin.
In the explanation of the process herein before given, the details of weights
employed represent those proportions which form the basis of the process. A small
alteration in the proportionate quantities given falls of course within the spirit of
the invention, that is to say, small modifications must not be considered as
constituting another process.

page_text: I, ADOLF BLAILE, of 24, Hafnerstrasse, Zurich, in the Republic of Switzerland,
Manufacturer, 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 has for, its object an improved process for the manufacture of
'artificial musk.
This process is carried out as follows:-
i
100 parts by weight of terpinol are mixed with 100 parts of ethyl, alcohol
(96% spirit) so that a clear solution of both substances results. The 200 parts of
solution obtained are poured into 1000 parts by weight of sulphuric acil of
66° Beaumé with constant stirring and cooling of the latter, and after the
completion of the pouring in, the mixture is vigorously stirred for 6 hours
further.
The sulphuric acid compound obtained by the above operations is gradually
poured into a quantity of 1000 parts by weight of concentrated nitric acid. free
from.chlorine, the necessary care being observed. It is necessary for this that the
nitric acid should be maintained in constant movement by stirring and the
temperature for the nitric acid should preferably not exceed 8° Celsius. After
these operations have been terminated, the mixture is warmed for about 4 hours
to 70° (or about 70°) Celsius and then cooled down and poured into 20,000 parts
by weight of water, which is vigorously stirred during the admixture. 'It forms
then an amorphous clear brown deposit, which is obtained by filtration.
The clear brown deposit obtained is pressed, dried and preferably made into
the form of cakes and constitutes the new perfume in a crude condition. For
the purpose of obtaining the perfume pure, the brown cakes obtained in the
nanner herein before described are ground to a fine powder and treated with
hot water until a sample of the brown mud dissolved with alcohol shows, a neutral
.reaction.
This last mentioned substance (mud) is filtered and 'dried and repeatedly purified
by means of suitable solvents, such, for instance, as petroleum-ether, until a clear
yellow crystalline substance is obtained. This latter has a delicate agreeable musk
scent.and.is used in perfumery.
It must also be mentioned that by the process herein before described, a musk-
smelling crystalline substance is obtained, if, instead of the terpinül mentioned at
the commencement of the specification, an equal quantity by weight of turpentine
oil or eucalyptus oil or the oils of fossil resins, as for instance oil of amber, retene
oil or the like be employed, or another body which shows the chemical character
of the so-called; terpin.
In the explanation of the process hereinbefore given, the 'details of weights
employed represent those proportions which form the-basis of the process. A small
alteration in the proportionate quantities given falls of course within the spirit of
the invention, that is to say, small modifications must not be considered as
constituting-another process.
.
Having now particularly described and ascertained the nature of my said inven-
tion and in what manner the same is to be performed, I declare that what I
claim is :-
Aprocess for producing derivatives of the terpin series' smelling of musk, which
consists in dissolving the terning in eleabal nausing the colution ind

page_text: acid, then the latter mixture into nitric acid, and finally the whole into water,
whereby the crude-musk-smelling substance is deposited in the water as a brown
amorphous mass, substantially as herein before set forth.
Dated this 11th day of January 1897.
WM. P. THOMPSON & Co.,
Of 6 Lord Street, Liverpool, Agents for the Applicant.