反应详情

To a flask charged with N2 was added 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}-3,6-dihydropyridine-1(2H)-carboxylate (424 mg, 0.629 mmol, 1.0 eq) followed by glacial acetic acid (40 mL). To this solution was added platinum oxide (42 mg, 10% w/w). The reaction solution was evacuated via vacuum and replaced with nitrogen (5×). The reaction mixture was then evacuated again via vacuum and placed under 1 atm of hydrogen and was allowed to stir for 17 hours. The solution was filtered through a pad of celite, washed with acetic acid and concentrated. The crude concentrate was dissolved in EtOAc and washed with saturated sodium bicarbonate. The organic layer was dried (Na2SO4), filtered, condensed, and purified via flash chromatography (1:1 tetrahydrofuran/hexanes). The purified fractions were collected, evaporated, and left under vacuum overnight to yield the title compound (320 mg, 75.3% yield). 1H-NMR (DMSO-d6) MS [M+H]+=676; LCMS RT=3.52 min.

1. customThe reaction solution was evacuated via vacuum
2. customThe reaction mixture was then evacuated again via vacuum
3. filtrationThe solution was filtered through a pad of celite
4. washwashed with acetic acid
5. concentrationconcentrated
6. concentrationThe crude concentrate
7. dissolutionwas dissolved in EtOAc
8. washwashed with saturated sodium bicarbonate
9. dry with materialThe organic layer was dried (Na2SO4)
10. filtrationfiltered
11. customcondensed
12. custompurified via flash chromatography (1:1 tetrahydrofuran/hexanes)
13. customThe purified fractions were collected
14. customevaporated
15. waitleft under vacuum overnight