Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Methyl iodide | HCID 6328 | — |
| Edukt | Potassium Carbonate | HCID 11430 | — |
| Edukt | 4-Hydroxy-1-indanone | HCID 590547 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | 4-methoxy-2,3-dihydro-1H-inden-1-one | HCID 4547491 | — |
Reaktionsschritte
Methyl iodide (69 ml) is added dropwise over a period of 15 minutes to a stirred mixture of 4-hydroxy-1-indanone (150 g) and anhydrous potassium carbonate (154 g) dissolved in DMF (1.5 liter) cooled to 0° C. under nitrogen. The reaction mixture is stirred at RT for 24 hours and partitioned between methylene chloride and water. The methylene chloride fraction is washed with water and 2% aqueous NaOH and dried over Na2SO4. The dried extract is filtered, concentrated in vacuo and the residue dissolved in hot methanol which upon cooling forms a precipitate. The precipitate is filtered and recrystallized from methanol yielding the methoxy product as a solid, M.P. 104°-106° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US04588719 |
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| Quelldatensatz | uspto-grants-1986_05 |
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| ORD ID | ord-0d932194cf3c4aefb55369fad0a4e158 |
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| Quellennotiz | uspto-grants-1986_05 |
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