Phosphorus sulfide (P2S5) → HCID 23453664, compound

Participants

Reaction Steps

33 mmoles of 3-phenyl-spiro[bicyclo[2.2.2]-octane-2,2'-pyrrolidin]-5'-one are dispersed in 200 ml of toluene, and a mixture of 7.3 g of phosphorus pentasulfide and 7 g of calcium oxide is added, whilst stirring, and the mixture is stirred at 50° C. for 21/2 hours. The hot reaction solution is filtered into a saturated sodium carbonate solution. The residues are dissolved in concentrated hydrochloric acid and the solution is diluted with water and carefully combined with the toluene/sodium carbonate mixture. The aqueous phase is extracted several times with toluene and the extracts are combined, dried and concentrated in vacuo. Recrystallization of the residue from a little ethyl acetate gives colorless crystals.

Provenance & Evidence