反应详情

温度

0 °C

To a solution of cold (−5° C.) nitric acid (2.7 mL) was added concentrated sulfuric acid (1.75 mL, 32 mmoL) dropwise keeping the temperature below 5° C. The solution was added to a cooled solution of 2,6-difluoro-4-methoxy benzaldehyde (5.0 g, 29 mmoL) in sulfuric acid (20 mL) over 15 minutes keeping the temperature below 5° C. After stirring at 0° C. for 2 hours the orange solution was poured on to ice, the white precipitate which formed was collected by filtration to give the title compound as a white solid (6.33 g, 100%). 1H NMR (CDCl3) 10.20 (1 H, t, J=1.17 Hz), 6.69 (1 H, dd, J=11.68, 1.93 Hz), 4.03 (3 H, s).

1. customthe temperature below 5° C
2. customthe temperature below 5° C
3. additionwas poured on to ice
4. customthe white precipitate which formed
5. filtrationwas collected by filtration