反应详情

温度

70 °C

To a solution of 5-amino-1H-1,2,4-triazole-3-carboxylic acid (3.9 g, 30.45 mmol) in methanol (100 ml) was added SOCl2 (12 g, 100.84 mmol). The resulting solution was stirred for 48 h at 70° C. The resulting mixture was concentrated under vacuum, dissolved in water (100 ml), the pH was adjusted to 8 with NaHCO3 solution, and then extracted with dichloromethane (3×50 ml). The organic layer was dried over anhydrous magnesium sulfate and concentrated under vacuum to afford methyl 5-amino-1H-1,2,4-triazole-3-carboxylate as a white solid (800 mg, 65%).

1. concentrationThe resulting mixture was concentrated under vacuum
2. dissolutiondissolved in water (100 ml)
3. extractionextracted with dichloromethane (3×50 ml)
4. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
5. concentrationconcentrated under vacuum