An Improved Production of Artificial Musk.
Year: 1896

page_text: Date of Application, 30.h Jan., 1896
Complete Specification Left, 30th Nov., 1896-Accepted, 30th Jan., 1897
PROVISIONAL SPECIFICATION.
An Improved Production of Artificial Musk.
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:-
A new benzene sulphonic acid is a trimethylmethanedimethylbenzenesulphonic-
are mixed together
Vessel.
To the sulphuric acid preparation (a) are added small quantities (about
10 grammes at a time) of the preparation (6) with continual stirring the addition
being carefully conducted so that the temperature does not rise materially beyond
8 to 10° C.
When the whole has thus been mixed, the mixture is allowed to stand in its cold
bath for some hours.
After this time the mixture is poured very cautiously in small quantities into a
vessel containing about 7-2 litres of cold water, which operation requires great
caution on account of the intense heat which is developed by the mixing. This
mixture is allowed to stand for 12 hours and the oily layer which has collected upon
the surface is taken off the solution below the oily layer being poured into a
vessel containing 29.5 litres of a clear solution of coarse salt of 24° Beaum., and
well mixed for half an hour. The vessel is then covered and allowed to stand for

page_text: 48 hours. The crystals which have meanwhile formed are then collected on a
filter, pressed and crystallized from water and dried on a water bath. A crystalline
product is thus obtained having a creamy colour and consisting of trimethyl-
methanedimethylbenzenesulphonic-acid
An improved Production of Artificial Musk.
I, JOHN WILLIAM MACKENZIE, of the Firm of Wheatley & 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 new benzenesulphonic acid is a trimethylmethanedimethylbenzenesulphonic
acid having the following constitution
(CH,),
CH, C(CH),
SO,H
It is prepared from the two following preparations
PREPARATION (a).
1050 grammes of ordinary sulphuric acid and
460 grammes of chemically pure sulphuric acid of 66 degrees Beaumé,
are mixed together in a suitable vessel surrounded by ice and water
for constantly maintaining a temperature of from 8 to 10 degrees
Centigrade.
PREPARATION (b).
130 grammes of trimethylmethane CH.(CH)
90 grammes of dimethylbenzene C,H(CH,), liquid, boiling at 137° C.
70 grammes oil of turpentine
20 grammes of ethylbenzene C,H,C,H, boiling at 134° C.
10 grammes of dimethylethylmethane CH(CH,),C,H, (isopentan)

page_text: To the sulphuric acid preparation (a) are added small quantities (about
10 grammes at a time) of the preparation (6) with continual stirring the addition
being carefully conducted so that the temperature does not rise materially
beyond 8 to 10 degrees Centigrade.
When the whole has thus been mixed, the mixture is allowed to stand in its
cold bath for some hours.
After this time the mixture is poured very cautiously in small quantities into
a vessel containing about 7.2 litres of cold water which operation requires great
caution on account of the intense heat which is developed by the mixing. This
mixture is allowed to stand for 12 hours and the oily layer which has collected
upon the surface is taken off, the solution below the oily layer being poured into a
vessel containing 29-5 litres of a clear solution of coarse salt of 24 degrees Beautné,
and well mixed for half an hour. The vessel is then covered and allowed to stand
for 48 hours. The crystals which have meanwhile formed are then collected on a
filter, pressed through a cloth, washed with water, heated in a water bath to
125 degrees Centigrade, filtered quickly whilst hot through a cloth. When cool
a crystalline product is thus obtained having a creamy colour and consisting of
trimethylmethanedimethylbenzenesulphonic acid.
(CHS),
C.H, C(CH,)
SO,H.
The sulphonic acid obtained as described is then nitrated as follows:-
200 grammes of the sulpho-acid is added to a mixture of 1250 grammes of
ordinary sulphuric-acid 66 degrees Beaumé and 1250 grammes concentrated fuming
nitric-acid sp. gr. 1-525, and the whole placed for 3-4 hours on a water bath,
washed in 6 to 7 times as much water, allowed to stand for half a day until crystals
have formed.
The crystals are filtered, washed already in the filter, pressed and re-crystallized
with 95 degrees alcohol.
It is neutralized with ammonia 25 degrees Beaume, filtered, pressed and dried.
The finished pure produce smells very intensely of musk.
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:
1. The improved production of the benzene sulphonic acid substantially according
to the process above described.
2. The improved production of artificial musk substantially according to the
process above described.
Dated this 30th day of November 1896.
WHEATLEY & MACKENZIE,
40 Chancery Lane, London, W.C., Agents.