反应详情

温度

50 °C

A suspension of the sodium salt of 2-dimethoxymethyl-3-hydroxy-acrylonitrile (3.94 g, 23.86 mmol) in hydrochloric acid (20 ml, 0.5 M) is heated at 50° C. for 30 minutes. Excess hydrochloric acid is neturalized using triethylamine, before adding cyanoacetothioamide (2.39 g, 23.9 mmol) and a catalytic amound of benzyltrimethylammonium hydroxide. The mixture is stirred at room temperature for two hours, heated at 60° C. for 2 hours and then refluxed for 4 hours. Evaporation of the solvents leaves a solid that is purified on silicagel to yield 3,5-dicyano-2-marcaptopyridine.

1. temperatureheated at 60° C. for 2 hours
2. temperaturerefluxed for 4 hours
3. customEvaporation of the solvents
4. customleaves a solid
5. customthat is purified on silicagel
6. customto yield 3,5-dicyano-2-marcaptopyridine