Abstarct: In this research work, A triple four-component Ugi reaction of isocyanide, amine, aldehyde, and trimesic acid as the acid component with three acidic functional groups in MeOH at reflux conditions has been disclosed. The process employs readily available and low-cost reagents, a convenient synthetic procedure, and mild reaction conditions for the synthesis of pharmacologically significant and structurally interesting compounds with several peptide groups, suitable for dendrimers and self-assembling. Substituents could be independently varied at three different positions. Also a double four-component Azido-Ugi reaction of isocyanide, TMSN3, aldehyde, and 4,4'-sulfonyldianiline with two amine functional groups in MeOH at reflux conditions has been described. The synthesis of pharmacologically and structurally interesting compounds with two 1,5-disubstituted tetrazole rings via a reaction from available and inexpensive reagents under a convenient process and mild reaction conditions has been reported. Modifications in the structure of the reaction product could be followed by varying the aldehyde or isocyanide component. The products are new and were confirmed by Mass, 1H NMR, HPLC and 13C NMR spectral studies. In this research work, A triple four-component Ugi reaction of isocyanide, amine, aldehyde, and trimesic acid as the acid component with three acidic functional groups in MeOH at reflux conditions has been disclosed. The process employs readily available and low-cost reagents, a convenient synthetic procedure, and mild reaction conditions for the synthesis of pharmacologically significant and structurally interesting compounds with several peptide groups, suitable for dendrimers and self-assembling. Substituents could be independently varied at three different positions. Also a double four-component Azido-Ugi reaction of isocyanide, TMSN3, aldehyde, and 4,4'-sulfonyldianiline with two amine functional groups in MeOH at reflux conditions has been described. The synthesis of pharmacologically and structurally interesting compounds with two 1,5-disubstituted tetrazole rings via a reaction from available and inexpensive reagents under a convenient process and mild reaction conditions has been reported. Modifications in the structure of the reaction product could be followed by varying the aldehyde or isocyanide component. The products are new and were confirmed by Mass, 1H NMR, HPLC and 13C NMR spectral studies. In this research work, A triple four-component Ugi reaction of isocyanide, amine, aldehyde, and trimesic acid as the acid component with three acidic functional groups in MeOH at reflux conditions has been disclosed. The process employs readily available and low-cost reagents, a convenient synthetic procedure, and mild reaction conditions for the synthesis of pharmacologically significant and structurally interesting compounds with several peptide groups, suitable for dendrimers and self-assembling. Substituents could be independently varied at three different positions. Also a double four-component Azido-Ugi reaction of isocyanide, TMSN3, aldehyde, and 4,4'-sulfonyldianiline with two amine functional groups in MeOH at reflux conditions has been described. The synthesis of pharmacologically and structurally interesting compounds with two 1,5-disubstituted tetrazole rings via a reaction from available and inexpensive reagents under a convenient process and mild reaction conditions has been reported. Modifications in the structure of the reaction product could be followed by varying the aldehyde or isocyanide component. The products are new and were confirmed by Mass, 1H NMR, HPLC and 13C NMR spectral studies.