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The relentless rise in cancer incidence has sparked an urgent quest for a treatment. For centuries, natural product resources have been the bedrock of medicinal and pharmaceutical industries, capturing the interests of researchers to explore more on the potential of natural products to treat illnesses. Above all, β-carbolines derived from alkaloids are well-known for their various biological and pharmacological properties. In this work, we review the methodologies to synthesize 3,9-disubstituted β-carbolines framework through Pictet–Spengler, metal-catalysed cross-coupling, and multicomponent reactions. In addition, this study aims to investigate how the structural modifications affect their biological activities, with an emphasis on anticancer and antibacterial properties. Besides, the modifications at the C-3 and N-9 positions were evaluated for efficiency and selectivity towards 3,9-disubstituted β-carbolines. This article also highlighted the adaptability of 3,9-disubstituted β-carbolines scaffolds for further use in drug development.
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