Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Hydrazine | HCID 9321 | — |
| Edukt | N-(3-(6-chloro-5-cyano-4-(4-phenoxyphenyl)pyridin-2-yl)phenyl)acetamide | HCID 86665685 | — |
| Lösungsmittel | Isopropanol | HCID 3776 | — |
| Produkt | HCID 178474120 | HCID 178474120 | 41% |
Reaktionsschritte
A mixture of N-(3-(6-chloro-5-cyano-4-(4-phenoxyphenyl)pyridin-2-yl)phenyl)acetamide (25 mg, 0.057 mmol) and 35% aqueous hydrazine (0.051 mL, 0.568 mmol) in 2-propanol (1.5 mL) was heated to 160° C. under microwave for 1 h then cooled to room temperature. Purification with reverse phase HPLC (Sunfire S10 30×250 mm column), eluting with 60-90% solvent B (10% methanol-90% water-0.1% TFA) in solvent A (90% methanol-10% water-0.1% TFA), gave Example 25 as the faster eluting peak (18 mg, 41% yield, yellow solid) and Example 24 as the slower eluting peak (3 mg, 8% yield, yellow solid).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US08846673B2 |
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| Quelldatensatz | uspto-grants-2014_09 |
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| ORD ID | ord-bd940899d13e459c8c56ca64cf48df97 |
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| Quellennotiz | uspto-grants-2014_09 |
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