反应详情

温度

2 °C

Under argon, 5 g (19.3 mmol) of 2-aminomalononitrile-4-toluenesulfonate was initially charged in 50 g of methanol. 4.09 g (22.7 mmol) of sodium methoxide solution (30%) was added and the mixture was stirred at 2° C. for 2 hours. After neutralization with 0.204 g (3.4 mmol) of acetic acid, 3.6 g (19.9 mmol) of methylglyoxal solution (40%) was added. The mixture was stirred at 40° C. for 2 hours and then, at 20° C., 9.2 g (80 mmol) of hydrochloric acid (32%) was added and the mixture was stirred at 20° C. for 6 hours. The solvent was distilled off and the methyl 3-methoxy-5-methylpyrazine-2-carboxylate was extracted with methylene chloride. This gave 1 g of methyl 3-methoxy-5-methylpyrazine-2-carboxylate. The yield was 27 percent Other data concerning the title product was:

1. stirringThe mixture was stirred at 40° C. for 2 hours
2. stirringthe mixture was stirred at 20° C. for 6 hours
3. distillationThe solvent was distilled off
4. extractionthe methyl 3-methoxy-5-methylpyrazine-2-carboxylate was extracted with methylene chloride