反应详情

To a solution of (1S,3R)—N1-[5-fluoro-2-[5-fluoro-1-(p-tolylsulfonyl)pyrrolo[2,3-b]pyridin-3-yl]pyrimidin-4-yl]cyclohexane-1,3-diamine, 44e, (0.089 g, 0.178 mmol) in DMF (1.5 mL) was added methyl 2-chlorooxazole-4-carboxylate (0.031 g, 0.195 mmol), followed by DBU (0.029 mL, 0.195 mmol). The reaction mixture was allowed to stir at room temperature overnight. The reaction was warmed to 75° C. and allowed to stir for 3 hours. Added an additional 16 mg of the chlorooxazole ester and the reaction was heated at 75° C. overnight. The mixture was diluted into water and EtOAc. The layers were separated and the organic phase was washed with brine, dried over MgSO4, filtered and evaporated to dryness. The crude residue was purified by silica gel chromatography (0-20% MeOH/CH2Cl2) to afford 28 mg of desired product: LCMS RT=3.73 (M+1) 624.12.

1. temperatureThe reaction was warmed to 75° C.
2. stirringto stir for 3 hours
3. temperaturethe reaction was heated at 75° C. overnight
4. customThe layers were separated
5. washthe organic phase was washed with brine
6. dry with materialdried over MgSO4
7. filtrationfiltered
8. customevaporated to dryness
9. customThe crude residue was purified by silica gel chromatography (0-20% MeOH/CH2Cl2)