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This book deals with the synthesis of a series of novel calix[4]arene and calix[4]resorcinarene compounds and their characterization. The synthesis of calixarenes and calixresorcinarene compounds were carried out by the following procedure. (1) Synthesis of novel azo calix[4]arenes and azo calix[4]resorcinarene dyes by linking various aromatic amine to calix[4]arene and calix[4]resorcinarene through a diazo-coupling reaction. (2) Synthesis of para sulphonato calix[4]resorcinarene by treating formaldehyde and sodium sulfite to calix[4]resorcinarene. (3) Synthesis of lower rim substituted calix[4]arene were carried out by substituting phenyl urea to calix[4]arene. The compounds were purified and characterized by elemental analysis, FT-IR, UV-VIS, 1H NMR, 13C NMR, ESI- MS and FAB-MASS.