Phosphorus sulfide (P2S5) → HCID 12617938, compound

Participants

Reaction Steps

A mixture of 6.0 g. of 5,10-dihydro-11H-pyrrolo[2,1-c]-[1,4]benzodiazepin-11-one (Example 1), 2.64 g. of phosphorus pentasulfide and 50 ml. of pyridine is stirred and heated at the reflux temperature for 4 hours, and concentrated to remove the pyridine. The residue is treated with 75 ml. of 5% aqueous sodium bicarbonate solution and 5 ml. of methanol and stirred at room temperature overnight. The product crystallizes gradually and is collected, washed with water and dried. This crude product is dissolved in chloroform, passed through a bed of Magnesol® silica gel, and the solvent evaporated to give yellow crystals of 5,10-dihydro-11H-pyrrolo[2,1-c][1,4]benzodiazepin-11-thione, m.p. 228°-231°.

Provenance & Evidence