反应详情

2-[3,5-bis(trifluoromethyl)phenyl]-N-[6-[(7S,9aS)-7-({[(1,1-dimethylethyl)(dimethyl)silyl]oxy}methyl)hexahydropyrazino[2,1-c][1,4]oxazin-8(1H)-yl]-4-(5-fluoro-2-methylphenyl)-3-pyridinyl]-N,2-dimethylpropanamide (D56, 110 mg) was dissolved in dry MeOH (2 mL), cooled in an ice-salt bath before adding cHCl solution (0.2 mL), and stirring at R.T. for 2 hours. Poured directly onto a 5 g SCX column. Washed with MeOH (2×10 mL), before eluting the compound with NH3 in MeOH 94×10 mL). Solvent evaporated. Residue purified on a 5 g sek-pak column eluting with Pent to EtOAc to 10% MeOH/EtOAc. Solvent evaporated to afford the title compound as a white solid.

1. temperaturecooled in an ice-salt bath
2. additionPoured directly onto a 5 g SCX column
3. washWashed with MeOH (2×10 mL)
4. washbefore eluting the compound with NH3 in MeOH 94×10 mL)
5. customSolvent evaporated
6. customResidue purified on a 5 g sek-pak column
7. washeluting with Pent to EtOAc to 10% MeOH/EtOAc
8. customSolvent evaporated