反应详情

温度

70 °C

o-Nitrobenzaldehyde (20.4 g, 0.135 mol), formic acid (20.3 mL, 0.539 mol) and malonic acid (18.3 g, 0.176 mol) were stirred at 45° C. for half an hour. Then ammonium formate (21.3 g, 0.338 mol) was added thereto, the reaction temperature was raised to 70° C. and stirred for 1 hour, and then stirred at 95° C. for another 4 hours. Then concentrated hydrochloric acid (50 mL) was added and further stirred maintaining this temperature for another 1 hour. It was cooled. 25 mL water was added, and washed twice with ethyl acetate (2×25 mL). The aqueous phase was adjusted to pH 4.2 with 50% potassium hydroxide solution. A solid precipitated. It was pumping filtered, and dried in vacuum to obtain a yellow solid 18.33 g, at a yield of 64.6%.

1. stirringstirred at 95° C. for another 4 hours
2. stirringfurther stirred
3. temperaturemaintaining this temperature for another 1 hour
4. temperatureIt was cooled
5. washwashed twice with ethyl acetate (2×25 mL)
6. customA solid precipitated
7. filtrationIt was pumping filtered
8. customdried in vacuum