HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl iodide → 4-methoxy-2,3-dihydro-1H-inden-1-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 4-Hydroxy-1-indanone | HCID 590547 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 4-methoxy-2,3-dihydro-1H-inden-1-one | HCID 4547491 | — |
Reaction Conditions
| Temperature | 0 °C |
|---|
Reaction Steps
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.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04699906 |
| Source dataset | uspto-grants-1987_10 |
| ORD ID | ord-199a2fb1ff564d64b775b69167c04b6b |
| Source note | uspto-grants-1987_10 |