反应详情

温度

0 °C

A 100 mL dry flask under a nitrogen atmosphere was charged with NaH (60% in mineral oil, 186 mg, 4.65 mmol). The NaH was washed with pentane (5 mL), THF (2 mL) was added, and the reaction was cooled to 0° C. The title compound from Example 21 (651 mg, 4.65 mmol) in THF (3 mL) was added dropwise, after which 15-crown-5 (1.41 mL, 7.12 mmol) was added. The reaction was allowed to warm to room temperature and stirred for 10 minutes, and then was cooled to 0° C. again. A solution of the title compound from Example 22 (1.19 mmol, used directly from the previous reaction) in THF (2 mL) was added, and the reaction was stirred at room temperature overnight.

1. customA 100 mL dry flask under a nitrogen atmosphere
2. washThe NaH was washed with pentane (5 mL), THF (2 mL)
3. additionwas added
4. temperatureto warm to room temperature
5. temperaturewas cooled to 0° C. again
6. additionwas added
7. stirringthe reaction was stirred at room temperature overnight