Coupling of various phenyl pyrazolone derivatives with diazonium salt of 1H-benzo[g]pyrazolo[3,4 b]quinoline-3-ylamine gave a series of heterocyclic azo compounds. All the synthesized azo compounds have been characterized by their percentage yield, elemental, and spectral analyses. These new compounds were evaluated for their in vitro antibacterial activity against Staphylococcus aureus, Bacillus subtilis, Escherichia coli, and Pseudomonas aeruginosa. Furthermore, the synthesized compounds were tested for in vitro antituberculosis activity against Mycobacterium tuberculosis. Streptomycin, Isoniazid, Rifampicin, and Ethambutol were used as standards in this investigation.