Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Methanesulfonic Acid | HCID 6395 | — |
| Edukt | Safinamide | HCID 131682 | — |
| Lösungsmittel | Ethyl Acetate | HCID 8857 | — |
| Produkt | Safinamide Mesylate | HCID 3038502 | 99,2% |
Reaktionsschritte
A mixture of (S)-2-[4-(3-fluorobenzyloxy)benzylamino]propanamide (20 g, 66 mmol, prepared in Example 12a) and ethyl acetate (510 g) is heated, under stirring up to 65° C. and kept under these conditions until a clear solution is obtained. Methanesulfonic acid (7 g, 72.6 mmol) is added in 40 min to the solution precooled to 55° C. The mixture is gradually cooled to 20° C. in 3 hours, kept at 20° C. for 2 hours. The heterogeneous mixture is filtered, the solid is dried at reduced pressure at 40° C. to yield 26.1 g of title compound as white powder (99% yield).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US08846763B2 |
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| Quelldatensatz | uspto-grants-2014_09 |
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| ORD ID | ord-0f665efc78a44a52ab336c047df35c59 |
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| Quellennotiz | uspto-grants-2014_09 |
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