In this chapter, Isoxazole is the parent substance of a large group of heterocyclic compounds, and these compound play a vital role in biological processes. A brief review regarding their spectral characteristics, general methods of systhesis was presented. The chalcone synthesized (earlier and reported) in present work, has now been taken for the preparation of corresponding new isoxazole derivatives. Refluxing with hydroxylamine hydrochloride in the in the presence of potassium hydroxide in ethanol, resulted in the formation of corresponding isoxazole (V) derivative. The purification and charactersation of isoxazole was presented.