反应详情

温度

70 °C

4-Fluoro-2-nitrobenzaldehyde (16.91 g, 0.10 mol), formic acid (15.2 mL, 0.40 mol) and malonic acid (13.52 g, 0.13 mol) were stirred at 45° C. for half an hour, and then ammonium formate (15.76 g, 0.25 mol) was added thereto. The reaction temperature was raised to 70° C. and stirred for 1 hour, and then stirred at 9° C. for another 4 hours. Then concentrated hydrochloric acid (38 mL) was added and stirred maintaining this temperature for another 1 hour. It was cooled, water (20 mL) was added, and extracted with ethyl acetate (2×25 mL). The organic phase was discarded, the aqueous phase was adjusted to pH≈4.2 with 50% potassium hydroxide solution. A solid precipitated, pumping filtered, dried in vacuum to obtain a yellow solid 16.71 g, at a yield of 73.2%.

1. stirringstirred at 9° C. for another 4 hours
2. stirringstirred
3. temperaturemaintaining this temperature for another 1 hour
4. temperatureIt was cooled
5. extractionextracted with ethyl acetate (2×25 mL)
6. customA solid precipitated
7. filtrationpumping filtered
8. customdried in vacuum