In the first part of this thesis, a green and efficient one pot multi- component protocol has been developed for the synthesis of some novel symmetrical bis-spirooxindole derivatives from the reaction of isatins, dihalides, C-H activated carbonyl compounds and malono derivatives in the presence of potassium carbonate (K2CO3) in polyethylene glycol (PEG-400) as a biodegradable polymeric solvent at room temperature. In this research, a variety of symmetrical bis-spirooxindole derivatives were obtained with excellent yields within short reaction time and without chromatographic separation. In another study, a simple and elegant synthesis of some novel bis -spiro pyranopyrazoles has been achieved via the condensation reaction between bis-isatins, malononitrile, hydrazine hydrate and ß -ketoester derivatives in the presence of a catalytic amount of 1, 4 -diazabicyclo [2.2.2] octane (DABCO) in ethanol at reflux conditions. The significant features of the present method are structure diversity, product complexity, procedure and work -up simplicity, environmentally friendly, good to excellent yields and catalyst recyclability. In another part of this thesis, a ligand-free Cu-catalyzed synthesis of vinyl sulfides derivatives via the reaction between aryl (alkyl) iodides or bromides with potassium iso-propyl zanthate (68) as sulfur transfer reagent and phenyl acetylene is described. In the last part of this thesis, a catalyst free method for sulfenylation of 3,4-dihydro-2H-pyran (DHP) via one-pot reaction between thiol or diaryl/dialkyl disulfide or aryl halide and DHP at 70 oC is reported.