反应详情

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0 °C

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-methyl-3,4′-bipyridin-3′-yl}-N,2-dimethylpropanamide (D53, 86 mg) was dissolved in dry MeOH (4 mL), cooled in an ice/salt bath to ˜0° C. before adding c.HCl solution. The mixture was stirred at ˜0° C. for 45 mins before allowing to warm up to R.T. and stirring for a further 2 hrs. Placed on a 5 g SCX column, washed with MeOH×3, before eluting compound off with NH3 in MeOH. Solvent evaporated. Residue purified on a 5 g sek pak column eluting with Pent to EtOAc to 10% MeOH/EtOAc. Solvent evaporated to dryness in vacuo to afford a colourless gum of the title compound.

1. additionbefore adding c
2. temperatureto warm up to R.T.
3. stirringstirring for a further 2 hrs
4. washwashed with MeOH×3
5. washbefore eluting compound off with NH3 in MeOH
6. customSolvent evaporated
7. customResidue purified on a 5 g sek pak column
8. washeluting with Pent to EtOAc to 10% MeOH/EtOAc
9. customSolvent evaporated to dryness in vacuo