反应详情

The mixture of N-cyano-N'-{2-[(4-methyl-5-imidazolyl)methylthio]ethyl}-S-methylisothiourea (10.0 g; 0.0371 mole) and distilled propargylamine (20 ml; 0.325 mole) in methanol (50 ml) was stirred at reflux, under a positive pressure nitrogen atmosphere (nitrogen sweep), for 20.5 hours. The solvent and excess amine were then removed by evaporation to leave a yellow-brown oil that readily crystallized. Trituration of the crude product under isopropanol (30 ml) gave the title compound as an off-white, friable solid (8.11 g, 79%); m.p. 146°-148.5°.

1. temperatureat reflux, under a positive pressure nitrogen atmosphere (nitrogen sweep), for 20.5 hours
2. customThe solvent and excess amine were then removed by evaporation
3. customto leave a yellow-brown oil that
4. customreadily crystallized