HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
3-Bromo-5-phenylpyridine → Ethyl 6-hydroxy-6-(5-phenyl-3-pyridinyl)-3-azabicyclo[3.2.1]octane-3-carboxylate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 3-Bromo-5-phenylpyridine | HCID 2762904 | — |
| Edukt | Ethyl 6-oxo-3-azabicyclo(3.2.1)octane-3-carboxylate | HCID 53302214 | — |
| Edukt | HCID 178418918 | HCID 178418918 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | Ethyl 6-hydroxy-6-(5-phenyl-3-pyridinyl)-3-azabicyclo[3.2.1]octane-3-carboxylate | HCID 57486356 | 14,2% |
Reaktionsschritte
To a solution of 3-bromo-5-phenylpyridine (0.23 g, 1.0 mmol) in THF (5 mL) at ambient temperature was added 2.0 M isopropylmagnesium chloride in THF (0.5 mL). The reaction was stirred for an hour under nitrogen. Then a solution of ethyl 6-oxo-3-azabicyclo[3.2.1]octane-3-carboxylate (0.21 g, 1.0 mmol) in THF (2 mL) was added. The mixture was stirred at ambient temperature overnight, concentrated and quenched with water (1 mL). The mixture was extracted with chloroform (2×10 mL), and the combined extracts were dried over magnesium sulfate, filtered, and concentrated by rotary evaporation. The compound was purified by silica gel column chromatography (1:1 ethyl acetate/hexane) to yield 50 mg of product (13%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07402592B2 |
| Quelldatensatz | uspto-grants-2008_07 |
| ORD ID | ord-89737a3b41aa4b4ca0bdba7e3185248c |
| Quellennotiz | uspto-grants-2008_07 |