HCID 54412353, compound → HCID 12687103, compound

Participants

Reaction Conditions

Reaction Steps

To 1.0 g of 2-chloro-6-(p-fluorophenylthio)phenyl-acetic acid was added 10 g of polyphosphoric acid and the resulting mixture was stirred at 150° C. for 2 hours. After cooling, to the mixture was added water and the mixture was extracted with benzene. The extract was washed with water, dried over anhydrous sodium sulfate and freed of solvent under reduced pressure. The residue obtained was recrystallized from benzene-n-hexane to afford 0.55 g (58.8%) of 2-fluoro-9-chloro-10,11-dihydrodibenzo[b,f]thiepin-11-one as colorless crystals having a melting point of 135°-137° C.

Provenance & Evidence