Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrazine | HCID 9321 | — |
| Reactant | HCID 58959717 | HCID 58959717 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 178487769 | HCID 178487769 | — |
Reaction Steps
6-Methoxy-3-oxo-2,7-dihydro-3H-pyrido[4,3,2-de]phthalazine-8-carboxylic acid hydrozide (39) To a suspension of 38 (0.45 g, 1.54 mmol) in EtOH (20 mL) was added hydrazine (1 mL) at room temperature. The reaction mixture was heated at 68° C. for 1.5 h and then cooled to room temperature. The resulting precipitate was filtered and washed with Et2O to afford a white solid (39, 0.31 g, 74%). 1H NMR (DMSO-d6, 300 MHz) δ 10.5 (br s, 1H), 9.0 (br s, 1H), 7.15-7.25 (m, 2H), 7.1 (br s, 1H), 6.8 (br s, 1H), 4.90 (br s, 2H), 4.03 (s, 3H). Mp: 305-307° C.; Anal. Calcd for C12H11N5O3.(0.75H2O): C, 50.26; H, 4.39; N, 24.42. Found: C, 50.33; H, 4.46; N, 22.04.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07601719B2 |
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| Source dataset | uspto-grants-2009_10 |
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| ORD ID | ord-249602fc9d834ba785cdc7f2cf0f763c |
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| Source note | uspto-grants-2009_10 |
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