反应详情

A mixture of 0.88 g. of 7-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 mixture is concentrated to dryness and the residue is stirred in 20 ml. of 1 N sodium carbonate solution (pH 7-7.2) for 18 hours. The precipitate is collected, washed with water and recrystallized from methanol-water to give a deep yellow solid, m.p. 197°-198.5° C. (dec.).

1. additionA mixture of 0.88 g
2. temperatureheated
3. temperatureunder reflux for 4 hours
4. concentrationThe mixture is concentrated to dryness
5. customThe precipitate is collected
6. washwashed with water
7. customrecrystallized from methanol-water
8. customto give a deep yellow solid, m.p. 197°-198.5° C. (dec.)