Hydrochloric Acid → Dibenzo[b,f][1,4]thiazepine-11(10H)-thione

Reaktionsgleichung

P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:2].[CH:15]1[C:20]2[C:21](=O)[NH:22][C:23]3[CH:29]=[CH:28][CH:27]=[CH:26][C:24]=3[S:25][C:19]=2[CH:18]=[CH:17][CH:16]=1.Cl>N1C=CC=CC=1>[CH:15]1[C:20]2[C:21](=[S:2])[NH:22][C:23]3[CH:29]=[CH:28][CH:27]=[CH:26][C:24]=3[S:25][C:19]=2[CH:18]=[CH:17][CH:16]=1

Komponenten

Versuchsvorschrift

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).