Attempts to prepare 2,4-bisthiosemicarbamoylpentanediones 1 via litera
ture precedent from 2,4-pentanedione and three different thiosemicarba
zides resulted instead in the formation of cyclic pyrazolines 5. The p
reparation was attempted with thiosemicarbazide, 4-methylthiosemicarba
zide, and 4-ethylthiosemicarbazide, respectively. A single-crystal X-r
ay structure study of the product from 4-methylthiosemicarbazide confi
rmed the pyrazoline structure. This observation serves to correct earl
ier misassignments of structure.