Acetone → Bazedoxifene Acetate

Participants

Reaction Conditions

Reaction Steps

Bazedoxifene free base (18 g) and acetone (162 mL) are mixed and stirred at 45-55° C. to make a clear solution. The said solution is cooled to room temperature and filtered to make particle free. To the filtrate, seed crystals of bazedoxifene acetate (360 mg) are added at room temperature and mixture is cooled to 15-20° C. followed by addition of a solution of acetic acid (2.34 g) in acetone (18 mL) at the same temperature. To the mixture, heptane (486 mL) is added over a period of 5-10 minutes and mixture is stirred at 15-20° C. for solid formation. The solid so obtained is collected by filtration and washed with heptane (50 mL) and dried under vacuum at below 80° C. to afford 17.80 g of crystalline bazedoxifene acetate Form D. D90=76.17 microns; D10=3.58 microns, D50=33.59 microns. The material is subjected to micronization under nitrogen atmosphere with a pressure of 4 kg/cm2 to afford the particles with D90=12.32 microns; D10=1.11 microns, D50=4.19 microns.

Provenance & Evidence