反应详情

温度

0 °C

To a solution of the product of Example 1B (0.220 g, 1.0 mmol) and the product of EXAMPLE 1C (0.268 g, 1.0 mmol) in anhydrous THF (10 mL) under nitrogen at 0° C. was added sodium hydride (95%, 0.10 g, 4.0 mmol). The reaction was heated to reflux for 3 hours, cooled to 0° C., and to it was added dropwise glacial acetic acid (2 mL). The resulting mixture was heated to reflux for 2 hours, cooled to ambient temperature, and diluted with aqueous hydrochloric acid (0.1 M, 10 mL). The resulting precipitate was collected by filtration, washed with water and diethyl ether and dried to give the title compound (0.130 g, 33%). MS (ESI−) m/z 397 (M−H)−.

1. temperatureThe reaction was heated
2. temperatureto reflux for 3 hours
3. temperatureThe resulting mixture was heated
4. temperatureto reflux for 2 hours
5. temperaturecooled to ambient temperature
6. filtrationThe resulting precipitate was collected by filtration
7. washwashed with water and diethyl ether
8. customdried