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ChemicalBook CAS DataBase List 1,4-DIAMINO-5-NITROANTHRAQUINONE

1,4-DIAMINO-5-NITROANTHRAQUINONE synthesis

3synthesis methods
1,4-Diamino anthraquinone? in oblate sulfuric acid.
-

Yield:-

Reaction Conditions:

with sulfuric acid

Steps:

1 EXAMPLE 1

EXAMPLE 1 60 g of sulphur trioxide are added dropwise over the course of 15 minutes to 150 g of sulpholane. At the conclusion of the addition the temperature is 30°-40°C. With stirring, 23.8 g of 1,4-diaminoanthraquinone are added and the batch is kept for 4 hours at 60°-65°C. and then cooled to 20°C-25°C. At this temperature 16.5 g of 50% mixed nitric and sulphuric acid are added dropwise over the course of 2 hours and stirring is continued for 4 hours. The precipitated crystallized 5-nitro-1,9-4,10-anthraquinone-disulphonimide is filtered off, washed with water and dried. The yield is 74.5% of theory. The 1,4-diamino-5-nitroanthraquinone is obtained from the nitroanthraquinone-disulphonimide in known manner, e.g. by saponification with 96% sulphuric acid at 120°C.

References:

US3978095,1976,A

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