Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Dimethylformamide | HCID 6228 | — |
| Edukt | Potassium Carbonate | HCID 11430 | — |
| Edukt | 4-Acetylpyridine | HCID 14282 | — |
| Edukt | (Benzyloxycarbonylmethyl)triphenylphosphonium bromide | HCID 11214019 | — |
| Lösungsmittel | Diethyl Ether | HCID 3283 | — |
| Produkt | Benzyl 3-(4-pyridyl)-2-butenoate | HCID 67118931 | 42,4% |
Reaktionsschritte
N,N-Dimethylformamide (33 ml) was added to a mixture of 4-acetylpyridine (2.00 g, 16.5 mmol) and (benzyloxycarbonyl)methyltriphenylphosphonium bromide (8.94 g, 18.2 mmol), and the whole was stirred under ice-cooling. Potassium carbonate (9.12 g, 66.0 mmol) was added thereto, the external temperature was raised to 70° C., and the whole was stirred overnight. The reaction mixture was diluted with diethyl ether (100 ml), and the whole was washed with water (100 ml, twice) and saturated brine (50 ml) successively. The organic layer was dried over magnesium sulfate and concentrated under reduced pressure. The residue was purified by silica gel column chromatography to give 1.77 g (42%: mixture of E form and Z form) of benzyl 3-(4-pyridyl)-2-butenoate as a pale yellow oily matter.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US07098226B2 |
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| Quelldatensatz | uspto-grants-2006_08 |
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| ORD ID | ord-0be49fb58b2f4f039baba09b76a48389 |
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| Quellennotiz | uspto-grants-2006_08 |
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