Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Ethanol | HCID 702 | — |
| Edukt | Piperidine | HCID 8082 | — |
| Edukt | Methyl (3r,4s)-1-[(z)-1-(methylthio)-2-nitrovinyl]-4-[(3r)-3-phenylpyrrolidin-1-yl]carbonylpiperidine-3-carboxylate | HCID 67304566 | — |
| Produkt | HCID 67304657 | HCID 67304657 | 71% |
Reaktionsschritte
To a stirred solution of methyl (3R,4S)-1-[(Z)-1-(methylthio)-2-nitrovinyl]-4-[(3R)-3-phenylpyrrolidin-1-yl]carbonylpiperidine-3-carboxylate (81.0 mg, 0.000187 mol) in ethanol (3.0 mL, 0.051 mol) was added piperidine (92.8 uL, 0.000934 mol). The reaction mixture was heated to reflux (oil bath temperature: 85° C.) for 17 h 45 min. The reaction mixture was concentrated in vacuo. The residue was purified by Combiflash with 0-8% MeOH/CH2Cl2 to give the product as a yellow solid (62 mg, 71% in yield). MS (ESI): (M+H)+=471.1.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US08853243B2 |
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| Quelldatensatz | uspto-grants-2014_10 |
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| ORD ID | ord-86d0059da46f4c7b8d0dce17ee575e2e |
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| Quellennotiz | uspto-grants-2014_10 |
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