Claims
- 1. A one-batch process for the manufacture of dianthraquinonyl-N,N'-dihydroazine, which comprises reacting 1-nitroanthraquinone in a mixture of (a) water or a mixture of water and at least one alcohol and (b) an alkali metal hydroxide or a mixture of alkali metal hydroxides at a temperature of between room temperature and the boiling temperature of the reaction mixture with hydrazine, hydrazine hydrate, methyl hydrazine, ethyl hydrazine, phenyl hydrazine, hydrazinium chloride, hydrazinium dichloride, hydrazinium sulfate, hydrazinium bromide, benzenesulfonyl hydrazine, hydroxylamine, hydroxylamine hydrochloride, hydroxylammonium sulfate or hydroxylamine sulfonic acid, subsequently removing any alcoholic constituents present from the reaction mixture, adding to the reaction mixture dimethyl sulfoxide or dimethyl sulfoxide and a further amount of alkali metal hydroxide, and bringing the reaction to completion at a temperature between 80.degree. and 140.degree. C.
- 2. A process according to claim 1, wherein the reaction of 1-nitroanthraquinone with hydrazine or hydroxylamine compound as defined in claim 1 is carried out at the boiling temperature of the reaction mixture with reflux cooling.
- 3. A process according to either of claim 1 or claim 2, wherein any alcoholic constituents present are removed from the reaction mixture by distillation.
- 4. A process according to either of claim 1 or claim 2, wherein the reaction is brought to completion in the temperature range of between 120.degree. to 125.degree. C.
- 5. A process according to either of claim 1 or claim 2, wherein the reaction is brought to completion while introducing air.
- 6. A process according to either of claim 1 or claim 2, wherein about equal amounts of water and alcohol are used.
- 7. A process according to either of claim 1 or claim 2, wherein there are used about equal parts of alkali metal hydroxide and 1-nitroanthraquinone, and, based on the 1-nitroanthraquinone, about twice the molar amount of the hydrazine or hydroxylamine compound as defined in claim 1.
- 8. A process according to either of claim 1 or claim 2, wherein the reaction of 1-nitroanthraquinone with hydrazine or hydroxylamine compound as defined in claim 1 is carried out in a mixture of water, methanol or ethanol and potassium hydroxide.
- 9. A process according to either of claim 1 or claim 2, wherein two to three times the initial amount of alkali metal hydroxide is added after removal of any alcoholic constituents present from the reaction mixture.
- 10. A process according to either of claim 1 or claim 2, wherein dimethyl sulfoxide is employed in an amount about as great as the amount of water and alcohol initially used.
- 11. A process according to either of claim 1 or claim 2, wherein hydrazine hydrate or hydroxylamine hydrochloride is used.
Priority Claims (1)
Number |
Date |
Country |
Kind |
4960/78 |
May 1978 |
CHX |
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Parent Case Info
This application is a continuation of application Ser. No. 149,125, filed May 8, 1980, which application is in turn a continuation of application Ser. No. 33,406, filed Apr. 6, 1979 (both now abandoned).
US Referenced Citations (3)
Non-Patent Literature Citations (1)
Entry |
Mosley, Chem. Ind. (London), (1959), pp. 1348-1349. |
Continuations (2)
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Number |
Date |
Country |
Parent |
149125 |
May 1980 |
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Parent |
33406 |
Apr 1979 |
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