関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 1,4-Phthalazinedione, 2,3-dihydro-5-nitro- | HCID 3525223 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 3-Nitrophthalic anhydride | HCID 21631 | — |
| 生成物 | Hydrazine hydrate (1:1) | HCID 24654 | — |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08536171B2 |
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| 出典データセット | uspto-grants-2013_09 |
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| ORD ID | ord-42f5c4ec241d47c49c82ad8761e19773 |
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| 出典メモ | uspto-grants-2013_09 |
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