HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Potassium Iodide → 7-hydroxy-6-(1-methylethoxy)-2H-1-benzopyran-2-one
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Potassium Iodide | HCID 4875 | — |
| Edukt | 2-Bromopropane | HCID 6358 | — |
| Edukt | Potassium Carbonate | HCID 11430 | — |
| Edukt | 7-(benzyloxy)-6-hydroxy-2H-chromen-2-one | HCID 1204535 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | 7-hydroxy-6-(1-methylethoxy)-2H-1-benzopyran-2-one | HCID 19927640 | — |
Reaktionsschritte
50.0 g (186 mmol) 6-hydroxy-7-phenylmethoxy-2H-1-benzopyran-2-one, 36.3 ml (387 mmol) isopropylbromide, 51.5 g (373 mmol) potassium carbonate and 5.0 g potassium iodide are agitated in 500 ml DMF for 14 h at 80° C. After filtration the filtrate is evaporated and the product recrystallized from isopropanol, yield: 57.7 g (100%) 6-(1-methyl-ethoxy)-7-(phenylmethoxy)-2H-1-benzopyran-2-one. Of this 50.0 g (161 mmol) are agitated in 100 ml of glacial acetic acid and 90 ml concentrated hydrochloric acid for 2.5 h at 70° C. This is followed by evaporation and purification using column chromatography on silica gel (eluent: chloroform and methanol 98/2 H 95/5): 24.65 g (69%), fusion point 121°-122° C. (from isopropanol).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05428038 |
| Quelldatensatz | uspto-grants-1995_06 |
| ORD ID | ord-747befdf939047769ae78720d23bd309 |
| Quellennotiz | uspto-grants-1995_06 |