Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Thiosemicarbazide | HCID 2723789 | — |
| Reactant | Phthalazine-5-carboxylic acid | HCID 57991901 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 57991941 | HCID 57991941 | 63% |
Reaction Steps
To a 100 mL round bottom flask was added phthalazine-5-carboxylic acid (0.50 g, 2.9 mmol) 1,1′-carbonyldiimidazole (0.93 g, 5.7 mmol) and DMF (2.2 mL). The mixture was stirred at 70° C. for 1 hour and treated with thiosemicarbazide (0.81 g, 8.9 mmol). The resulting mixture was stirred at 70° C. for 30 minutes. The mixture was concentrated under vacuum to remove almost all of the DMF. The remaining residue was treated with 2 N HCl with stirring until the solution reached pH 4. Upon standing, a yellow solid formed. The precipitate was recovered by filtration, washing with water and air dried to provide 1-(phthalazine-5-carbonyl)thiosemicarbazide (0.45 g, 63%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07919504B2 |
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| Source dataset | uspto-grants-2011_04 |
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| ORD ID | ord-a1f3af060daf44efad8482c81b17d8c5 |
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| Source note | uspto-grants-2011_04 |
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