反应详情

温度

60 °C

To a suspension of compound 22 (100 mg, 0.25 mmol) in glacial acetic acid (2 mL) at room temperature was added nitric acid (0.1 mL, d 1.35) dropwise with vigorous stirring. The mixture was heated at 60° C. for 3 h, left to cool for 30 min, and poured into cold water. The resulting precipitate was filtered and recrystallized to afford compound SKC-BF-11 (50 mg, 49%) as an orange solid. TLC Rf=0.6 (CHCl3-MeOH, 9:1); 1H NMR (CDCl3) δ 7.90 (s, 1H), 7.13 (s, 2H), 3.95 (s, 3H), 3.88 (s, 6H); MS (ES) m/z 411 (M+H)+.

1. waitleft
2. temperatureto cool for 30 min
3. filtrationThe resulting precipitate was filtered
4. customrecrystallized
5. customto afford compound SKC-BF-11 (50 mg, 49%) as an orange solid