Cyclization of ethyl 2,4-dioxovalerate (I) with 3-(trifluoromethyl)phenylhydrazine (II) in a refluxing mixture of HOAc and 2-methoxyethanol produced pyrazole ester (III). After saponification of the ethyl ester group of (III), the resulting carboxylic acid (IV) was coupled to 5-aminoisoquinoline (V) by using O-(7-azabenzotriazol-1-yl)-N,N,N',N'-tetramethyluronium hexafluorophosphate to furnish the corresponding amide.