反应详情

To a flask charged with tert-butyl 4-{4-amino-5-[3-fluoro-4-({[2-fluoro-5-(trifluoromethyl)phenyl]carbamoyl}amino)phenyl]-6-(methoxymethyl)pyrrolo[2,1-f][1,2,4]triazin-7-yl}piperidine-1-carboxylate was added methylene chloride (12.5 mL). To this suspension was added 12.5 mL of trifluoroacetic acid. The homogeneous solution was allowed to stir at rt under nitrogen for 17 hours. The reaction mixture was concentrated and the residue dissolved in EtOAc. The organic phase was washed with saturated sodium bicarbonate solution (2×), brine (1×), separated and the organic layer dried (Na2SO4). The organic layer was filtered, concentrated and left under vacuum overnight to yield the title compound (150 mg, 70.4% yield). 1H-NMR (DMSO-d6) MS [M+H]+=576; LCMS RT=2.51 min.

1. concentrationThe reaction mixture was concentrated
2. dissolutionthe residue dissolved in EtOAc
3. washThe organic phase was washed with saturated sodium bicarbonate solution (2×), brine (1×)
4. customseparated
5. dry with materialthe organic layer dried (Na2SO4)
6. filtrationThe organic layer was filtered
7. concentrationconcentrated
8. waitleft under vacuum overnight