反应详情

Phosphorus pentasulphide (1.2 eq) was added to a solution of 10,11-dihydrodibenzo[b,f][1,4]thiazepin-11-one (1.14 g, 5 mmol) in pyridine (40 ml) and heated under reflux for 15 hr. The mixture was allowed to cool and poured into hydrochloric acid (1.3M) at 0° C. Filtration of the yellow precipitate and purification by chromatography on silica (eluting with dichloromethane/methanol, 99:1) followed by recrystallisation from ethanol gave the title compound as yellow crystals (700 mg, m.p. 245°-246° C., Rf 0.81, CH2Cl2/MeOH9:1).

1. temperatureheated
2. temperatureunder reflux for 15 hr
3. temperatureto cool
4. filtrationFiltration of the yellow precipitate and purification by chromatography on silica (eluting with dichloromethane/methanol, 99:1)
5. customfollowed by recrystallisation from ethanol