6-Hydroxybuspirone → Buspirone

Participants

Reaction Steps

Batch B. The remainder of the solution (water content 0.13%) was allowed to cool to ambient temperature and seeded with 6-hydroxybuspirone (20 mg) at approximately 56° C. The mixture was filtered seven days later on a 4-6 micron glass sintered filter and the reactor rinsed (four times with the mother liquor in order to recover all solids). The mother liquor was saved for analysis (620 mL). The off-white solid was subsequently washed with IPA (2×260 mL). The white solid was suctioned dried for 1 h and then placed into a an oven at 45° C. (27 in Hg with an N2 bleed for 69 hours). 6-Hydroxybuspirone was obtained as an off-white solid (156.6 g, AP=99, buspirone AP=0.35, and a trans-diol side product AP=0.54).

Provenance & Evidence