Hydrochloric Acid → Hydrochloric Acid

Participants

Reaction Steps

Using the same reaction procedure as in EXAMPLE 5, 14.25 g (48.3 mmoles) of 11b-(4-fluorophenyl)-1,3,4,6,7,11b-hexahydro-2H-benzo[a]quinolizin-2-one, along with 140 ml (2.16 M, 302 mmoles) of methanolic dimethylamine, 21 ml (5.0 N, 105 mmoles) of HCl and 3.0 g (47.7 mmoles) of NaBH3CN are rejected. Using the same work-up procedure as in EXAMPLE 5, 15.6 g (99%) of white crystals of 11b-(4-fluorophenyl)-1,3,4,6,7,11b-hexahydro-N,N-dimethyl-2H-benzo[a]quinolizin-2-amine is obtained. m.p. 158°-168° C. This product is converted to the hydrochloride salt by reaction with HCl in ethanol. The salt is recrystallized from butanone/methanol, producing a highly hydroscopic HCl salt as beige needles of 11b-(4-fluorophenyl)-1,3,4,6,7,11b-hexahydro-N,N-dimethyl-2H-benzo[a]quinolizin-2-amine dihydrochloride. After 3 subsequent recrystallizations, pink crytals are obtained. m.p. 293°-298° C. (dec.)

Provenance & Evidence