反应详情

Dissolve N-[(1R)-1-(4-{[(2S)-2-(4-fluorophenyl)morpholin-4-yl]methyl}phenyl)ethyl]methanesulfonamide (50 g, 127.39 mmol) in isopropyl alcohol (200 mL). Add HCl (4M in dioxanes; 63.70 mL, 254.78 mmol) drop-wise to the solution and stir at ambient temperature for 50 min. Remove the volatiles under reduced pressure; add H2O (200 mL); then evaporate the water. Add H2O (200 mL) and isopropyl alcohol (100 mL), and concentrate to a total volume of 80 mL. Filter the resulting thick slurry; wash solid with H2O; collect by filtration; and dry the filter cake under reduced pressure at 55° C. to provide the title compound as a white solid (40.6 g, 75%). MS (m/z): 393 (M-Cl).

1. customRemove the volatiles under reduced pressure
2. customthen evaporate the water
3. concentrationAdd H2O (200 mL) and isopropyl alcohol (100 mL), and concentrate to a total volume of 80 mL
4. filtrationFilter the resulting thick slurry
5. washwash solid with H2O
6. filtrationcollect by filtration
7. customand dry the filter cake under reduced pressure at 55° C.