反应详情

温度

90 °C

A stirring mixture of 4-hydroxypyridin-2(1H)-one (1.2 g, 10 8 mmol, prepared according to the procedure described at Step A of Example 8), tert-butyl 4-(methylsulfonyloxy)piperidine-1-carboxylate (4.83 g, 17 3 mmol, prepared according to the procedure described at Step C of Example 1) and potassium carbonate (3.13 g, 22 7 mmol) in DMF (45 mL) was heated at 90° C. for 14 hrs and then cooled to room temperature. The resulting mixture was diluted with EtOAc and H2O and the aqueous layer was extracted further with EtOAc (5×). The combined extracts were washed with brine, dried (Na2SO4) and evaporated under reduced pressure. The residual was purified by flash chromatography on silica gel (0 to 10% MeOH/CH2Cl2) to yield 1.23 g (38.7%) of the product as a pinkish solid. MS (ESI) 295 (M+H).

1. customprepared
2. customprepared
3. temperaturecooled to room temperature
4. extractionthe aqueous layer was extracted further with EtOAc (5×)
5. washThe combined extracts were washed with brine
6. dry with materialdried (Na2SO4)
7. customevaporated under reduced pressure
8. customThe residual was purified by flash chromatography on silica gel (0 to 10% MeOH/CH2Cl2)