反应详情

温度

0 °C

The crude compound from Step 1 was dissolved in tetrahydrofuran (500 mL), the solution was cooled to 0° C., and sodium hydride (as a 60% dispersion in oil, 9.4 g, 235 mmol) was added in portions. After stirring at 0° for 1 hour, the mixture was allowed to warm up to room temperature. After 2 hours, water (400 mL) was added to the suspension and and the insoluble solid was filtered and washed copiously with water. When dry, the solid was stirred in ether (150 mL) at room temperature for 24 hours and filtered to afford the title compound as a cream-colored solid.

1. temperatureto warm up to room temperature
2. waitAfter 2 hours
3. filtrationthe insoluble solid was filtered
4. washwashed copiously with water
5. customWhen dry
6. stirringthe solid was stirred in ether (150 mL) at room temperature for 24 hours
7. filtrationfiltered