反应详情

Batch A. Approximately 1000 mL was transferred to a vessel equipped with a magnetic stirrer and water was added (15 mL, Karl Fischer titration indicated 3.94% water). This solution was then slowly cooled to ambient temperature while stirring, and seeded with 6-hydroxybuspirone (approximately 20 mg). The mixture was filtered seven days later on a 4-6 micron glass sintered filter and the mother liquor saved for analysis (740 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 h). 6-Hydroxybuspirone was obtained as an off-white solid (166.0 g, purity=99 AP, buspirone AP=0.35, and a trans-diol side product AP=0.54).

1. customApproximately 1000 mL was transferred to a vessel
2. customequipped with a magnetic stirrer
3. filtrationThe mixture was filtered seven days later on a 4-6 micron glass
4. filtrationsintered filter
5. washThe off-white solid was subsequently washed with IPA (2×260 mL)
6. customThe white solid was suctioned dried for 1 h
7. customplaced into a an oven at 45° C.