反应详情

温度

0 °C

A solution of nitric acid (1.68 mL, 70%, 26. 8 mmol) in sulfuric acid (5 mL) was added dropwise to a 0° C. solution of Example 66A (3.27 g, 13.4 mmol) in sulfuric acic (15 mL). The resulting mixture was stirred at 0° C. for 1 hour, warmed to room temperature overnight, and poured into ice water. The resulting precipitate was collected by filtration, washed with water, and dried in a vacuum oven to provide 2.47 g (64% yield) of the desired product. MS (ESI(+)) m/e 290 (M+H)+.

1. temperaturewarmed to room temperature overnight
2. filtrationThe resulting precipitate was collected by filtration
3. washwashed with water
4. customdried in a vacuum oven