Hydrochloric Acid → 8,10-Dichloro-3,7-dimethoxy-10,11-dihydrodibenzo(b,f)-thiepine

Participants

Reaction Steps

Anhydrous hydrogen chloride was passed at 0° C. into a stirred solution of the alcohol from the above experiment (22.5 g) in methylene chloride (500 ml) for 3 hours. Anhydrous calcium chloride (5 g) was added, the mixture stirred at room temperature for 3 hours and filtered. The filtrate was evaporated under diminished pressure, yielding 23.4 g of crude 8,10-dichloro-3,7-dimethoxy-10,11-dihydrodibenzo(b,f)-thiepine. The compound was crystallized from methylene chloride and melted in the pure state at 151°-153° C.

Provenance & Evidence