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The present research work is divided into four chapters which mainly focusing on the development and application of novel protocols for the synthesis of various functionalized aryl nitriles, N-Boc protected amines, pyrazoles and quinoxalines. The first chapter deals with Catalyst-free, efficient and one pot protocol for synthesis of nitriles from aldehydes using glycerol as green solvent. This protocol was efficiently used for transformation of aromatic aldehydes bearing electron-withdrawing and electron-donating groups into aryl nitriles in good to excellent yields. The methodology offers a very simple, efficient and environmentally benign procedure. The second chapter deals with Catalyst-free, highly efficient and chemoselective N-tert-butyloxycarbonylation of amines in green solvent glycerol. The varieties of functionalized amines such as aliphatic, aromatic as well as heteroaromatic were protected by using developed protocol. The third chapter deals with Iodine promoted efficient synthesis of 3,5-Disubstituted 1H-pyrazoles from acetophenone hydrazone and substituted aldehydes. This practical one-pot protocol is metal-free and requires no isolation of less stable intermediate.