Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Acetic Acid | HCID 176 | — |
| Edukt | 4-[3-Chloro-4-(3-fluoro-benzyloxy)-phenylamino]-6-nitro-quinazoline | HCID 53630476 | — |
| Lösungsmittel | Methanol | HCID 887 | — |
| Produkt | Allitinib metabolite M6 | HCID 53630477 | 61% |
Reaktionsschritte
In a flask equipped with a reflux condenser, the compound obtained in Example 6 1.60 g (3.77 mmol), reduced iron powder 1.05 g (18.85 mmol, 5 eq), glacial acetic acid (2 mL) and methanol (40 mL) were mixed. The mixture was refluxed in an oil bath at a temperature of 85° C. for 2.5 h. Then the iron powder was filtered of, the filtrate was diluted with ethyl acetate, washed sequentially with NaHCO3 solution and water. The organic phase was dried and concentrated to obtain yellow solid, which was identified as the title compound. Yield: 61%.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US08044063B2 |
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| Quelldatensatz | uspto-grants-2011_10 |
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| ORD ID | ord-4858870967fe4189a60da34c0b585ad0 |
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| Quellennotiz | uspto-grants-2011_10 |
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