Bazedoxifene Acetate → Bazedoxifene

Participants

Reaction Conditions

Reaction Steps

Bazedoxifene acetate (47 g) and dimethylformamide (235 mL) are mixed and heated to 80° C. to produce a clear solution, followed by filtration. To the filtrate, toluene (2700 mL), morpholine (3.0 mL), and water (1810 mL) are added and the mixture is stirred overnight at room temperature. The solid is collected by filtration, washed with toluene (70 mL) and water (70 mL), then dried under vacuum below 80° C. for about 6-8 hours to afford Form A of crystalline bazedoxifene free base: D90=49.80 microns; D10=3.61 microns, D50=25.30 microns. The material is subjected to micronization under nitrogen atmosphere with a pressure of 4 kg/cm2 to afford the particles with D90=6.04 microns; D10=0.89 microns, D50=2.37 microns.

Provenance & Evidence