Reaktion #77607

ord-3398eeb0de564ba9ab1b8cc49873e73a

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe mixture is refluxed for 12 hours
  2. 2
    Temperaturcooled
  3. 3
    Filtrationfiltered
  4. 4
    EinengenThe filtrate is concentrated under reduced pressure
  5. 5
    Sonstigepurified by chromatography on a column of silica
  6. 6
    SonstigeA yellow oil is obtained (m=12.70 g; Y=73%)

Vorschrift

9.25 g (43.2 mmol) of 5-(2-ethyl-[1,3]dioxolan-2-yl)-2-thienylmethyl methanesulphonate are dissolved in 100 mL of 2-butanone, and 9.07 g (43.2 mmol) of dimethyl 4-hydroxyphthalate (prepared in Example 1(b)), 6 g of potassium carbonate (43.2 mmol) and 20 mg of sodium iodide are added. The mixture is refluxed for 12 hours, cooled and filtered. The filtrate is concentrated under reduced pressure and then purified by chromatography on a column of silica. A yellow oil is obtained (m=12.70 g; Y=73%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06706725B1uspto-grants-2004_03