A study was made of the thermal degradations of 1.4-disubstituted thiosemicarbazides of general formula R1-CH-/CO2R2/-NH-CS-NH-NH-R 3, which lead to the formation of cyclic 3-aminothiohydantoins. The rate of cyclization was determined by DTG and compared with the semiquantitative rcsults of DTA which are influence by the melting of the substances examined. The Rl-substituted 3-aminothiohydantoins produced by cyclization undergo further thermal decomposition, with evolution of hydrogen sulphide as a low-molecular volatile product and formation of a polymeric residue characterized by a considerable stability.