反应详情

温度

20 °C

2,2,5-Trifluoro-6-nitrobenzo[d][1,3]dioxole (2.5 g, 11 mmol) was dissolved in dry methanol (20 mL), treated with 30% sodium methoxide solution (3.1 g, 17 mmol), and stirred at 20° C. for 1 h. After excess methoxide was neutralized by addition of acetic acid, the volatiles were removed by rotary evaporation. The residue was taken up in ethyl acetate (50 mL), washed with saturated NaHCO3 (10 mL), saturated NaCl (10 mL), dried (Na2SO4) and evaporated. The material was purified by chromatography on silica with a 0-30% ethyl acetate-hexane gradient to give the title compound as a white solid (1.8 g, 70%): mp 84-85° C. 1H NMR (400 MHz, CDCl3) δ 7.71 (s, 1H), 6.89 (s, 1H), 3.98 (s, 3H); 19F NMR (376 MHz, CDCl3) δ −49.90 (s); EIMS m/z 233.

1. customthe volatiles were removed by rotary evaporation
2. washwashed with saturated NaHCO3 (10 mL), saturated NaCl (10 mL)
3. dry with materialdried (Na2SO4)
4. customevaporated
5. customThe material was purified by chromatography on silica with a 0-30% ethyl acetate-hexane gradient