Methanol → Bazedoxifene Acetate

Participants

Reaction Conditions

Reaction Steps

Crystalline bazedoxifene free base (1.7 Kg) is charged in a mixture of methanol (20.4 L) and isopropyl alcohol (13.6 L) and heated to reflux temperature to make a clear solution and stirred at same for 15-30 minutes. The solution is filtered and subsequently cooled to about 25-30° C. over a period of 10 minutes followed by addition of acetic acid (0.28 Kg) and seed crystals of Form D (85 g). Then the mixture is further allowed to cool to 0-5° C. over a period of about 20 minutes. The reaction mixture is maintained at the same temperature for 30-60 minutes and the solid is collected by filtration, washed with pre-cooled methanol (3.4 L), and dried under vacuum at about 60-65° C. to afford the title compound.

Provenance & Evidence