反应详情

3-[(3-Aminopropyl)amino]-N,N-dimethylbenzamide (0.8 g) and N-cyano-1-methyl-2 -(phenylmethylene)hydrazine carboximidothioic acid, methyl ester eluent (0.84 g) were heated together under reduced pressure of 14 mm Hg during 4 hr at 100°. The cooled reaction mixture was dissolved in acetone, treated with 1N hydrochloric acid (2 ml) and heated at 60° for 0.5 hr. The mixture was cooled, basified with potassium carbonate and extracted with ethyl acetate. Evaporation of the organic extracts gave a viscous oil which was triturated with ether to give the title compound (0.49 g). TLC silica; methanol:ammonia (80:1) Rf 0.63. NMR (CDCl3) 2.9 m (1H); 3.2-3.7 m (3H); 5.28 t (1H); 6.12 s (2H); 6.7 s (3H); 7.0 s (6H); 6.4-7.4 m (5H); 8.23 t (2H).

1. customThe cooled reaction mixture
2. temperatureheated at 60° for 0.5 hr
3. temperatureThe mixture was cooled
4. extractionextracted with ethyl acetate
5. customEvaporation of the organic extracts
6. customgave a viscous oil which
7. customwas triturated with ether