反应详情

温度

105 °C

Compound 67 (581.6 mg, 1.431 mmol) obtained in Example 63 was dissolved in tert-butanol (48 mL), and pyrimidium p-toluenesulfonate (3.6 g; 14 mmol) was added thereto, followed by stirring at 105° C. for 4 hours. The reaction mixture was cooled to 0° C., a saturated aqueous ammonium chloride solution was added, followed by extraction with ethyl acetate (50 mL×3). The organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate, and concentrated to yield a residue. The residue was purified by silica gel column chromatography, followed by purification by high-speed liquid chromatography (60 to 100% acetonitrile/water) to obtain the title compound (150 mg, 29%).

1. temperatureThe reaction mixture was cooled to 0° C.
2. extractionfollowed by extraction with ethyl acetate (50 mL×3)
3. washThe organic layer was washed with saturated brine
4. dry with materialdried over anhydrous magnesium sulfate
5. concentrationconcentrated
6. customto yield a residue
7. customThe residue was purified by silica gel column chromatography
8. customfollowed by purification by high-speed liquid chromatography (60 to 100% acetonitrile/water)