Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | 4-Fluoropiperidine | HCID 2759159 | — |
| Edukt | HCID 59262218 | HCID 59262218 | — |
| Lösungsmittel | Acetonitrile | HCID 6342 | — |
| Produkt | HCID 59262163 | HCID 59262163 | 103,1% |
Reaktionsschritte
A mixture of 1,1-dimethylethyl (2S)-4-({4-[[(6-bromo-3-pyridinyl)carbonyl](methyl)amino]phenyl}methyl)-2-methyl-1-piperazinecarboxylate (D108) (0.050 g, 0.0993 mmol), 4-fluoropiperidine (0.055 g, 0.397 mmol) and triethylamine (0.069 mL, 0.497 mmol) in acetonitrile (4 mL) was heated at 85° C. overnight then in a microwave at 140° C. for 10 h. Further portions of 4-fluoropiperidine (5 eq.) and triethylamine (5 eq.) were added and the reaction heated at 170° C. for 2 h. The reaction mixture was concentrated and the residue dissolved in DCM/water. The aqueous layer was further extracted with DCM (×3) and the combined organics were dried (Na2SO4) and concentrated to give the title compound as a yellow oil (0.0538 g). MS (ES): MH+ 526.2.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US08853218B2 |
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| Quelldatensatz | uspto-grants-2014_10 |
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| ORD ID | ord-7180b9bf3dbd4204acb22909d7d1e44c |
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| Quellennotiz | uspto-grants-2014_10 |
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