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"Experimental Techniques in Medicinal Chemistry and Instrumental Methods" is a comprehensive practical guide designed for pharmacy students and professionals. It integrates core laboratory techniques in organic chemistry with essential instrumental methods used in pharmaceutical analysis. The book is divided into two main sections: one focusing on the synthesis, purification, and identification of organic compounds, and the other covering instrumental techniques such as UV-Vis spectroscopy, IR, and chromatography. Each experiment includes clear objectives, step-by-step procedures, observations, and discussions to build both conceptual understanding and practical skills. Emphasis is placed on laboratory safety, analytical precision, and real-world applications. This manual is especially useful for BSC, MSC, B.Pharm and M.Pharm students, educators, and those working in pharmaceutical quality control, offering a solid foundation in experimental pharmaceutical chemistry.