反应详情

温度

0 °C

To a 20 mL round-bottom flask were added (S)-tert-butyl 4-(5-(1-((5-cyano-6-ethyl-2-(methylthio)pyrimidin-4-yl)amino)ethyl)-1-methyl-1H-pyrrolo[3,2-b]pyridin-6-yl)piperazine-1-carboxylate (78 mg, 0.145 mmol) in acetonitrile (1.5 mL) and water (1.5 mL) along with OXONE® (223 mg, 0.363 mmol) at 0° C. The reaction mixture was allowed to stir for 30 minutes at 0° C. and then for 3.5 hours at room temperature. LCMS indicated the reaction was mostly complete. The reaction mixture was diluted with EtOAc and washed with brine (3×). The combined organic layers were dried over MgSO4, filtered, and concentrated. The product was purified by column chromatography (ISCO 4 g, 30-100% EtOAc/hexane gradient) to give the title compound as a yellow oil. ESI-MS m/z [M+H]+ calc'd for C27H36N8O4S, 569. found 569.

1. waitfor 3.5 hours at room temperature
2. washwashed with brine (3×)
3. dry with materialThe combined organic layers were dried over MgSO4
4. filtrationfiltered
5. concentrationconcentrated
6. customThe product was purified by column chromatography (ISCO 4 g, 30-100% EtOAc/hexane gradient)