Abstract Refined synthetic procedure for preparation of 3, 5-diamino-1, 2, 4-thiadiazole and 2, 5-diamino-1, 3, 4-thiadiazole based on the reaction of dithiourea or amidinothiourea with hydrogen peroxide is developed. The optimal reagents ratio was found, and monitoring methods were developed. It resulted in the increase of the target product yield and in a shorter reaction time. On the basis of 2, 5-diamino-1, 3, 4-thiadiazole the alkylsubstituted 1 ...