Reaktion #736191

ord-a9ecdd0c7d1e458796e44f0887a2686f

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONtetryhydrofuran are added dropwise at -78°
  2. 2
    Temperaturis maintained below -60°
  3. 3
    TemperaturAfter 30 minutes at -78° the temperature is slowly raised to 0°
  4. 4
    Sonstigethe organic phase separated
  5. 5
    Waschenwashed
  6. 6
    Sonstigedried
  7. 7
    Einengenconcentrated under vacuum
  8. 8
    SonstigeThe residue is chromatographed (eluant: n-hexane)

Vorschrift

To a solution of 7 g of 7-methylbenzo[b]thiophene in abs. tetryhydrofuran are added dropwise at -78°, 30 ml of a 1.6M solution of n-butyllithium in hexane. After 20 minutes 5.5 g of perchloryl fluoride are introduced whereby the reaction temperature is maintained below -60°. After 30 minutes at -78° the temperature is slowly raised to 0°. The mixture is then mixed with water and the organic phase separated, washed, dried and concentrated under vacuum. The residue is chromatographed (eluant: n-hexane) to obtain the title compound as an oil.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04737516uspto-grants-1988_04