Phosphorus sulfide (P2S5) → HCID 21865382, compound

Participants

Reaction Steps

To a stirred solution of 2,8-dichloro-10,11-dihydro-dibenzo[a,d]cycloheptene-5-one (0.70 g, 2.53 mMol) in toluene (20 ml) were added phosphorus pentasulfide (1 eq, 561 mg) and hexamethyldisiloxane (1 eq, 0.54 ml). The mixture was heated 3 h at reflux and allowed to cool to room temperature. The mixture was filtered through a pad of silica gel (70 g) and washed through with 8:1 heptane/ethyl acetate. Evaporation of the solvent under reduced pressure afforded 2,8-dichloro-10,11-dihydro-dibenzo[a,d]cycloheptene-5-thione as a blue solid (710 mg, 95%) that was used without further purification.

Provenance & Evidence