反应详情

温度

10 °C

To a 2 l, 3-necked flask equipped with an efficient stirrer, reflux condenser, and thermometer was added 116 g (1.0 mole) of 5-amino-3-mercapto-1,2,4-triazole, 1 l of glacial acetic acid and 153 g (1.5 moles) of acetic anhydride. The mixture was heated to reflux (118°-120°) with stirring for 2 hours and then cooled to about 10° C. Recovery of the solids present by filtration and drying resulted in about 102 g (65 percent of theory) of the title compound, m.p. 326°-328° (dec.), a white, crystalline solid. A sample purified by washing with 2-propanol and drying melted at 336° C. (dec.). The carbon nmr spectrum of this compound was consistent with the assigned structure, having absorptions at 169.29, 164.99, 144.77, and 22.73 ppm as were the proton nmr spectrum, having an absorption at -2.00 ppm, and the elemental (C, H, and N) analysis.

1. customTo a 2 l, 3-necked flask equipped with an efficient stirrer
2. temperaturereflux condenser
3. temperatureThe mixture was heated
4. temperatureto reflux (118°-120°)
5. filtrationRecovery of the solids present by filtration
6. customdrying