Manufacture of Nitro Amido Anthraquinone.
Year: 1894

page_text: Date of Application, 16th July, 1894
Complete Specification Left, 16th Apr., 1895-Accepted, 18th May, 1895
ORAL CLICATION.
[Communicated from abroad by THE FARBWERKE, vormals MEISTER LUCIUS
& BRUNING, of Hoechst a/ Main, in the Empire of Germany, Chemical
Manufacturers.]
Manufacture of Nitro Amido Anthraquinone.
I, OLIVER IMRAY, of No. 28 Southampton Buildings, Chancery Lane, in the
County of London, Chartered Patent Agent, do hereby declare the nature of this
invention to be as follows:-
According to the expired German Patent No. 6526 diamido anthraquinone is
obtained by heating dinitro anthraquinone with aqueous ammonia under pressure.
By modifying the conditions there described, especially by the substitution of
alcoholic for aqueous ammonia it is possible, as has been formerly observed, to
obtain an amido nitro anthraquinone.
My foreign correspondents have now found that the same amido nitro anthra-
quinone may also be obtained by heating dinitro anthraquinone with the bisulphites
of the alkalies or alkaline earths in aqueous solution under pressure.
The method employed is the following:
1 part by weight of dinitro anthraquinone is well stirred up with from 6 to
12 parts by weight of commercial sodium bisulphite solution, and beated from two
to five hours under pressure to from 120° to 180° C. The raw material obtained is
washed with water and purified with alcohol. Amido nitro anthraquinone
crystallises from alcohol in small red crystals which melt approximately at 200° C.
and give, on analysis, results corresponding to the theory
Calculated
C 62-7 %
Found
63.1 °

page_text: manufacture of Anthraquinone.
I, OLIVER IMRAY, of No. 28 Southampton Buildings, Chancery Lane, in the
County of London, Chartered Patent Agent, 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 :-
According to the expired German Patent No. 6526 diamido anthraquinone is
obtained by heating dinitro anthraquinone with aqueous ammonia under pressure.
By modifying the conditions there described, especially by the substitution of
alcoholic for aqueous ammonia it is possible, as has been formerly observed, to
obtain an amido nitro anthraquinone.
My foreign correspondents have now found that the same amido nitro anthra-
quinone may also be obtained by heating dinitro anthraquinone with the bisulphites
of the alkalies or alkaline earths in aqueous solution under pressure.
The method employed is the following:
1 part by weight of dinitro anthraquinone is well stirred up with from 6 to
12 parts by weight of commercial sodium bisulphite solution, and heated from two
to five hours under pressure to from 120° to 180° C. The raw material obtained is
washed with water and purified with alcohol. Amido nitro anthraquinone
crystallises from alcohol in small red crystals which melt approximately at 200° C.
and give, on analysis, results corresponding to the theory
Calculated
C 62-7 %
H 2.98%
N 10.44%
Found
63.1%
3.2%
10.5 %
Nitro amido anthraquinone dissolves according to its degree of purity in
70 per cent. fuming sulphuric acid with from red to red violet colour, which on
standing for a long time becomes blue, while diamido anthraquinone dissolves with
a blue colour. It dissolves in concentrated sulphuric acid with feeble yellow red
colour and does not separate out on cooling.
Instead of sodium bisuphite, ammonium or calcium bisulphite may be employed.
Having now particularly described and ascertained the nature of this inven-
tion and in what manner the same is to be performed, I declare that what I
claim is :-
The manufacture of nitro amido anthraquinone by treating the dinitro-
anthraquinone obtained by nitrating anthraquinone in sulphuric acid solution with
the bisulphites of the alkalies or alkaline earths in aqueous solution under pressure.
Dated this 16th day of April 1895.
ABEL & IMRAY,
Agents for the Applicant.