反应详情

温度

-15 °C

Treat 4-[4-[4-(hydroxydiphenylmethyl)-1-piperidinyl]-1-hydroxybutyl]-α,α-dimethylbenzeneacetic acid hydrochloride hydrate (Form II) (5.00 g, 0.0083 mol) with methylethyl ketone (130 mL). Slowly add water (0.4 mL), filter through filter aid and wash the filter cake with methylethyl ketone (20 mL). Heat to reflux and distill off 75 mL of solvent, cool to −15° C. and collect by vacuum filtration. Wash with methylethyl ketone (2×10 mL) and vacuum dry at 60° C. to give the title compound (4.33 g, 97%); mp 196–198° C.

1. filtrationSlowly add water (0.4 mL), filter
2. filtrationthrough filter aid
3. washwash the filter cake with methylethyl ketone (20 mL)
4. temperatureHeat
5. temperatureto reflux
6. distillationdistill off 75 mL of solvent
7. filtrationcollect by vacuum filtration
8. washWash with methylethyl ketone (2×10 mL) and vacuum
9. customdry at 60° C.