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

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Reaction Steps

Powdered anhydrous calcium chloride (5 g) was added to a solution of the alcohol from the preceding preparation (7.6 g) in methylene chloride (100 ml) and anhydrous hydrogen chloride introduced into the suspension for 2 hours. The mixture was then allowed to stand overnight and filtered. The filtrate was evaporated, yielding 7.5 g of the desired 8,10-dichloro-3,7-difluoro-10,11-dihydrodibenzo(b,f)thiepine which is crystallized from cyclohexane. The pure compound melts at 118.5°-119.5° C.

Provenance & Evidence