Reaktion #736191
ord-a9ecdd0c7d1e458796e44f0887a2686f
Reaktionsgleichung
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1workup.ADDITIONtetryhydrofuran are added dropwise at -78°
- 2Temperaturis maintained below -60°
- 3TemperaturAfter 30 minutes at -78° the temperature is slowly raised to 0°
- 4Sonstigethe organic phase separated
- 5Waschenwashed
- 6Sonstigedried
- 7Einengenconcentrated under vacuum
- 8SonstigeThe 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.