Phosphorus sulfide (P2S5) → HCID 12521655, compound

Participants

Reaction Steps

A mixture of 0.88 g. of 6-chloro-4,9-dihydro-10H-thieno[3,4-b][1,5]benzodiazepin-10-one and 1.0 g. of phosphorus pentasulfide in 10 ml. of dry pyridine is stirred and heated under reflux for 4 hours. The reaction mixture is concentrated to dryness and the residue is stirred with 20 ml. of 1N sodium carbonate solution (pH 7-7.2) for 18 hours. The precipitate is collected, washed with water and recrystallized from methanol to give an orange solid, m.p. 235°-237° C. (dec.).

Provenance & Evidence