Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Acetic Acid | HCID 176 | — |
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | (R)-(1-(5,6-Diaminopyridin-2-yl)piperidin-3-yl)(pyrrolidin-1-yl)methanone dihydrochloride | HCID 89854051 | — |
| Edukt | Ethyl 1-(2-methoxyphenyl)cyclopropanecarbimidate hydrochloride | HCID 89854623 | — |
| Lösungsmittel | Ethanol | HCID 702 | — |
| Produkt | HCID 178489265 | HCID 178489265 | — |
Reaktionsschritte
To a solution of (R)-(1-(5,6-diaminopyridin-2-yl)piperidin-3-yl)(pyrrolidin-1-yl)methanone dihydrochloride (32 mg, 0.088 mmol) in ethanol (0.5 mL) was added triethylamine (50 μL, 1.42 mmol) and acetic acid (82 μL, 1.42 mmol). Then a solution of ethyl 1-(2-methoxyphenyl)cyclopropanecarbimidate hydrochloride (50 mg, 0.09 mmol) in ethanol (0.3 mL) was added and the reaction mixture was heated to 75° C. for 18 h. The solvent was removed under reduced pressure and the residue was partitioned between ethyl acetate and a saturated aqueous solution of sodium bicarbonate. The organic layer was washed with water, dried over sodium sulfate, filtered and concentrated under reduced pressure. The crude material was purified via HPLC to afford the title compound. MS (ESI+) (M+H) 446.1; HPLC retention time: 2.299 min (Method A).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US09296745B2 |
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| Quelldatensatz | uspto-grants-2016_03 |
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| ORD ID | ord-84626f47ca0e4f05820aa09b5cb92670 |
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| Quellennotiz | uspto-grants-2016_03 |
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