Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | 1,2-Dichloroethane | HCID 11 | — |
| Edukt | Oxamic Acid | HCID 974 | — |
| Edukt | Trifluoroacetic acid | HCID 6422 | — |
| Edukt | 1-Hydroxybenzotriazole | HCID 75771 | — |
| Edukt | HCID 178514300 | HCID 178514300 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | N-methyl-2-pyrrolidone | HCID 13387 | — |
| Produkt | HCID 178513834 | HCID 178513834 | — |
Reaktionsschritte
To a mixture of 6-hydrazinyl-3-phenylpyrido[2,3-b]pyrazin-2(1H)-one (3-3) (300 mg, 1.19 mmol), HOBt (218 mg, 1.42 mmol) and oxamic acid (130 mg, 1.42 mmol) in NMP (12 mL) was added EDC (272 mg, 1.42 mmol) at room temperature and the mixture was stirred for 30 min. After addition of TFA (0.091 mL, 1.19 mmol), the mixture was heated under microwave irradiation at 150° C. for 30 minutes. To a mixture was added water (60 mL) and the precipitate was collected by filtration to give 3-hydroxy-2-phenyl[1,2,4]triazolo[4′,3′:1,6]pyrido[2,3-b]pyrazin-9-carboxamide (9-1) as a yellow powder.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US08207169B2 |
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| Quelldatensatz | uspto-grants-2012_06 |
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| ORD ID | ord-66a85126e86f4012a368f42eb2537669 |
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| Quellennotiz | uspto-grants-2012_06 |
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