A Process or Processes for the Manufacture of Artificial Musk.
Year: 1890

page_text: This Print is in accordance with the Original Specification as it stands after-
Amendment (under Section 18 of the Patents, &c. Act, 1883) as
allowed by the decision of the Comptroller General of the 31st day of
January 1894.
COMPLETE SPECIFICATION (AMENDED).
A Process or Processes for the Manufacture of Artificial Musk.
I, Dr. FRIEDRICH VALENTINER, Manufacturing Chemist, of Plagwitz-Leipzig,
in the German Empire, do hereby declare the nature of my invention, and in what
manner the same is to be performed, to be particularly described and ascertained in
and by the following statement :—
According to repeated experiments, a substance closely resembling natural musk-
may be obtained by the following simple process :
Isobutyl-alcohol and xylene (xylol) are mixed together in quantities corre-
sponding to their chemical equivalents, and the mixture is gradually introduced
into concentrated sulphuric acid, care being taken, that the temperature of 45° C. is
not exceeded.
When the condensation has been completed, the whole mixture is introduced,
with the usual caution, into fuming nitric acid, it is then precipitated with water,
and washed, and the dinitro-compound thus obtained is purified by repeated
re-crystallisation from alcoholic solution. Instead of xylene, oil of turpentine or
cymene (cymol) may be employed.
For instance, if isobutyl-alcohol, isopropyl-alcohol, or iso-amyl-alcohol are mixed
with oil of turpentine, the mixture introduced into concentrated sulphuric acid, and
the product nitrated, dinitro-compounds are obtained, which can be used as a
substitute for musk.
1
The same result may be obtained by treating cymene and one of the alcohols
mentioned above, with concentrated sulphuric acid and nitrating the product of the
reaction. The artificial musk thus obtained is much cheaper, than that produced
by the methods hitherto known, and it has a more agreeable odour.
I have found, that the product obtained from aromatic hydrocarbons and alcohols
of the fatty series by means of concentrated sulphuric acid, consists of two new
bodies, that is, firstly, the newly formed hydro-carbon, and secondly, the sulpho-
acid of the same, which is soluble in water.
On the product of the mixture or of the reaction being introduced into water, one
portion collects on the surface in the shape of an oil, while the other portion enters
into solution as a sulpho-acid. After the oil has been removed, the aqueous solution
is mixed with a saturated solution of common salt, until the solution tends to
become cloudy. After some time, the whole liquid is found to be interspersed with
a crystalline mass, which is then separated by filtration, dried and introduced into
fuming nitric acid. After dilution with water, and on the addition of a saturated'
solution of common salt, the nitro-compound crystallises in the shape of brilliant
scales, which have a strong musk-odour and are soluble in water.

page_text: Having now particularly described the nature of my invention, and in what
manner the same is to be performed, I declare that I am aware of the Specification
of Schnaufer and Hupfeld's Patent No. 18521 A.D.. 1888, and I wish it to be
understood that I make no claim for anything described and claimed therein, but
what I'claim is
1. The process for the manufacture of artificial musk, which consists in mixing
equivalent quantities of iso-butyl-alcohol and xylene, introducing the mixture into
sulphuric acid, placing the whole mixture, after condensation, in fuming nitric acid,
precipitating and washing the product with water, and purifying the dinitro-
compound thus produced by repeated crystallisation from alcoholic solution,
substantially as described.
2. The modification of the process specified above, by using oil of turpentine or
cymene, instead of xylene.
3. The process for the manufacture of artificial musk, which consists in treating
the product of condensation of xylene, cymene,sor oil of turpentine, and isoamyl-,
isopropyl-, or isobutyl-alcohol obtained by means of concentrated sulphuric acid,
allowing the mixture to cool, introducing the whole mixture into concentrated nitric
acid for nitration, subsequently precipitating and washing the product, substantially
as described.
4. The process for the manufacture of artificial musk, which consists in producing
two new bodies; namely an oil and a sulpho-acid obtainable by the treatment of
certain alcohols and aromatic hydro-carbons with sulphuric acid, removing the
supernatant oil; mixing the sulpho-acid with saturated solution of salt; intro-
ducing the crystalline mass, produced by the last mentioned operation, into
fuming nitric acid, and recrystallising the nitro-compound thus obtained, by
adding a saturated solution of common salt, substantially as described.
5. The products obtained by the processes specified in Claims 1 to 4.
1000