Phosphorus sulfide (P2S5) → HCID 135848425, compound

Participants

Reaction Steps

12.1 g (0.05 mol) of 1,3-dihydro-5-phenyl-2H-thieno[2,3-e]-1,4-diazepin-2-one are heated to reflux for 35 minutes with 12.2 g (0.055 mol) of phosphorus pentasulphide in 400 ml of absolute pyridine, dry nitrogen being conducted through the solution. The solution is concentrated to 200 ml and the mixture separated on a 70 cm long column (φ3.5 cm) filled with 250 g of Silica gel [0.05 to 0.2 mm (Merck)]. The solution is concentrated under a vacuum and yields 1,3-dihydro-5-phenyl-2H-thieno[2,3-e]-1,4-diazepine-2-thione in the form of yellow crystals, melting point 208°-210° C.

Provenance & Evidence