Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Acetone | HCID 180 | — |
| Edukt | Pyrrolidine | HCID 31268 | — |
| Edukt | alpha-Hydroxyacetophenone | HCID 68490 | — |
| Lösungsmittel | Toluene | HCID 1140 | — |
| Produkt | 2,2-Dimethyl-chroman-4-one | HCID 7454290 | 21,6% |
Reaktionsschritte
Twenty five grams (25 g) of 2-hydroxyacetophenon, 10.7 g of acetone, and 5.5 g of pyrrolidine were added to 50 ml of toluene, and heated and refluxed. Twenty hours later, the temperature was returned to ambient temperature and the solvent was distilled off under reduced pressure, to which was added 100 ml of 1N hydrogen chloride. The extraction was carried out with 50 ml×3 of chloroform, followed by washing in water, drying over anhydrous magnesium sulfate, filtering off and condensation of the filtered solution. The residue was purified on a silica gel column the fraction containing the purified product were mixed together and the solvent therein was distilled off under reduced pressure to obtain 7 g of 3,4-dihydro-2,2-dimethyl-2H-benzo[b]pyran-4-one.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US05260444 |
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| Quelldatensatz | uspto-grants-1993_11 |
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| ORD ID | ord-82943bc94705456ea20fa2554590862c |
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| Quellennotiz | uspto-grants-1993_11 |
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