反应详情

To a solution of N-Isopropyl-1-[3-(4-pyridinylethynyl)phenyl]-1,4-dihydro[1,8]naphthyridin-4-one-3-carboxamide from EXAMPLE 3 in methylene chloride (36 mL/mmol) and methanol (3 mL/mmol) was added magnesium monoperoxyphthalate hexahydrate (MMPP, 3.6 eq) and the mixture was stirred at room temperature overnight. A further amount of MMPP (2 eq) was added and stirring was continued for 24 hours. The resulting mixture was filtered through a bed of celite, the filtrate was diluted with methylene chloride and washed with aqueous sodium bicarbonate and water. After drying, the organic phase was evaporated and the crude product was purified by chromatography on silica gel eluting with 10% methanol in methylene chloride to afford the title compound as a solid.

1. stirringstirring
2. waitwas continued for 24 hours
3. filtrationThe resulting mixture was filtered through a bed of celite
4. additionthe filtrate was diluted with methylene chloride
5. washwashed with aqueous sodium bicarbonate and water
6. customAfter drying
7. customthe organic phase was evaporated
8. customthe crude product was purified by chromatography on silica gel eluting with 10% methanol in methylene chloride