A New Method for Producing an Artificial Scent or Musk-like Substance.
Year: 1897

page_text: Date of Application, 27th Apr., 1897
Complete Specification Loft 26th Fab 1000
Accented
27th June 1000
Date of Application, 27th Apr., 1897
Complete Specification Loft 26th Fab 1000
Accepted, 27th
June, 190
1000
PROVISIONAL SPECIFICATION.
A New Method for Producing an Artificial Scent or Musk-like
Substance.
I, JOHN WILLIAM MACKENZIE, of the Firm of Wheatley and Mackenzie,
Engineers and Patent Agents, of 40, Chancery Lane, in the County of London,
do hereby declare the nature of this invention (a communication to me from
Charles Schmid, of 47, Boulevard Anspach, Brussels, in the Kingdom of Belgium)
to be as follows:-
The object of this invention is to produce a material or materials having the
odour of musk.
The method of preparation depends upon the oxidation of certain oily and wax-
like products obtained from several fossil resins, namely copal, amber and retin-
resin. The oxidiser used by preference is chromic acid, but other equivalent
agents may be employed.
Copal, amber or retin-resin are subjected to distillation by means of superheated
steam under pressure, a suitable enamelled pot being employed. The various
products of distillation are fractionated, the wax-like fraction and the specifically
heavy oil being used for the subsequent oxidation.
The distillation is facilitated by the addition to the resins enumerated, of a
quantity of magnesia just sufficient to render the fused mass feebly alkaline.
The oxidation is carried out as follows:-100 grammes of the heavy oil or wax-
like substance are mixed with one kilogramme of sulphuric acid of 66 B., the acid
being kept cold by a freezing mixture. 100 grammes of powdered potassium
bichromate are then gradually added, with constant stirring of the acid solution.
This operation should take about five hours. After the fluid has become cold and
has become more or less clear, it is filtered through an asbestos filter, it is neutralised
with a mixture of equal parts of ammonia and alcohol. If there is any excess
of ammonia this is removed by the addition of a drop or two of dilute sulphuric
acid.
The neutralised solution is then heated till all alcohol has been driven off.
The solution thus obtained possesses a delicate odour. The odorous matters are
separated from the solution by means of ether, in which they are soluble. They
are obtained by spontaneous evaporation of the ether in the form of an oily
substance.
Dated this 27th dow of Anal 1807

page_text: A New Method for Producing an Artificial Scent or Musk-like
Substance.
I, JOHN WILLIAM MACKENZIE, of the Firm of Wheatley and Mackenzie,
Engineers and Patent Agents, of 40, Chancery Lane, in the County of London,
do hereby declare the nature of this invention-a communication to me from
Charles Schmid, of 47, Boulevard Anspach, Brussels, in the Kingdom of Belgium-
and in what manner the same is to be performed, to be particularly described and
ascertained in and by the following statement:-
The object of this invention is to produce a material or materials having the
odour of musk.
The method of preparation depends upon the oxidation of certain oily and wax-
like products obtained from several fossil resins, such as Zanzibar copal, amber
and retin-resin, which by distillation yield a product known as amber camphor.
The oxidiser used by preference is-chromic acid, but other equivalent agents may
be employed.
Zanzibar copal, amber or retin-resin are subjected to distillation by means of
superheated steam under pressure, a suitable enamelled pot being employed... The
temperature employed is from 240 to 350 degrees centigrade and the pressure
about 1 atmosphere. The products of distillation coming off at a temperature
below 240 degrees C. are rejected, and those which come off at a higher temperature
are utilized. The various products of distillation so fractionated include wax-like
fractions known in commerce as amber camphor, and specifically heavy oils which
contain some amber camphor.
The distillation is facilitated by the addition to the resins enumerated, of a
quantity of magnesia just sufficient to render the fused mass feebly alkaline.
The oxidation is carried out as follows: The preparation being kept cold by a
freezing mixture until treated with ammonia as hereinafter described, a temperature
of from 8 to 10 degrees C. being sufficient, 100 grammes of the mixed heavy oil
and wax-like substance are mixed with one kilogramme of sulphuric acid of 66 B.,
and 100 grammes of powdered potassium bichromate are then gradually added with
constant stirring of the acid solution. This operation should take about five hours.
After the fluid has become cold and has become more or less clear, it is filtered
through an asbestos filter, and is neutralised with a mixture of equal parts of
ammonia and alcohol. If there is any excess of ammonia this is removed by the
addition of a drop or two of dilute sulphuric acid.
This neutralised solution is then heated till all alcohol has been driven off.
The solution thus obtained possess a delicate odour. The odorous matters are
separated from the solution by means of ether, in which they are soluble. They
are obtained by spontaneous evaporation of the ether in the form of an oily
substance.
In practice five lots may be treated at one time to obviate the waste of time
that would otherwise occur when neutralising with ammonia.
Having now particularly described and ascertained the nature of my said
invention, and in what manner the same is to be performed, I declare that what
I claim is:
1. The process for the production of an artificial scent or musk-like substance,
substantially as described.
2. The new substance which is the result of the process hereinbefore described.

page_text: 3. The new method of producing an artificial scent or musk-like substance by
an oxiding process, substantially as herein before described.
Dated this 26th day of January 1898.
WHEATLEY & MACKENZIE,
40, Chancery Lane, London, W.C., Agents.