Synthesis of 4,3,5-R(MeO)2C6H2CONHCONHR' (I) and 4,3,5-R(MeO)2C6H2CH:CHCONHCONHR' (II) was described. Urea (3.5 g.) and 4,3,5-EtO2CO(MeO)2C6H2COCl (6 g.) were warmed 2-3 hrs. under continuous stirring on the oil bath at 140-50°; the mass solidified with HCl development. After addition of H2O and overnight standing, the mixture was filtered and the residue recrystallized from EtOH to give I (R = EtO2CO, R' = H), m. 203-4°. Similarly the following compounds were prepared (general formula, R,R', m.p. given): I, EtO2CO, Me, 170-5° (MeOH); I, EtO2CO, Ph, 172-3° (EtOH); II, MeO, H, 218-19° (EtOH); II, MeO, Me, 224-5° (EtOH); II, MeO, Ph, 195-6° (EtOH); I, MeO, Ph, 150-1° (EtOH). The last compound was alternatively synthesized from 3,4,5-(MeO)3C6H2CONH2 and OCNPh by warming 2-3 hrs. at 150-60°. Urea (7.11 g.) and 3-Me2NC6H4COCl.HCl (13.35 g.) were warmed 2-3 hrs. on the oil bath, the resulting vitreous mass, dissolved in H2O, and neutralized with saturated NaHCO3 solution to give a precipitate of 3-Me2NC6H4CONHCONHR (III) (R = H), m. 190-1° (EtOH); hydrochloride m. 213-14°. Similarly the following III were prepared and recrystallized from EtOH (R and m.p. of III and their HCl salts given): Me, 139-40°, 193-4°; Ph, 176-7°, 203-4°. I, II, and III were obtained as crystals insoluble in H2O, soluble in the usual organic solvents. Pharmacol. screening of these compounds was under study.