Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Water | HCID 962 | — |
| Edukt | 1,4-Phthalazinedione, 2,3-dihydro-5-nitro- | HCID 3525223 | — |
| Lösungsmittel | Acetic Acid | HCID 176 | — |
| Produkt | 3-Nitrophthalic anhydride | HCID 21631 | — |
| Produkt | Hydrazine hydrate (1:1) | HCID 24654 | — |
Reaktionsschritte
where M is Li, Na, K wherein 5-nitro-2,3-dihydrophthalazine-1,4-dione is solved in water solution of MOH, where M has the above mentioned meaning, with forming solution of 5-nitro-2,3-dihydrophthalazine-1,4-dione alkaline salt which is catalytically transformed in 5-amino-2,3-dihydrophthalazine-1,4-dione salt at the temperature of 40-90° C. by means of hydrogen under the pressure of 1-4 MPa at the presence of a transition metal catalyst (Pt, Pd) on active carbon, and separation of 5-amino-2,3-dihydrophthalazine-1,4-dione crystalline salt is performed by dilution of the water solution with lower alcohol or cyclic lower ether while cooling to the temperature −5° C. to −15° C., providing that there is used 5-nitro-2,3-dihydrophthalazine-1,4-dione obtained in the reaction of 3-nitrophthalic acid anhydride with hydrazine hydrate in anhydrous acetic acid at the temperature 100-110° C. with distilling the mixture of acetic acid and water off.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US08536171B2 |
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| Quelldatensatz | uspto-grants-2013_09 |
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| ORD ID | ord-42f5c4ec241d47c49c82ad8761e19773 |
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| Quellennotiz | uspto-grants-2013_09 |
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