The book reported that the literature survey of the chemistry of three different types of photosensitizers as porphyrins, phthalocyanines and cyanine dyes. The development of one- pot reactions represents a great challenge in organic synthesis today. Indeed, this strategy allows the construction of highly complex molecules from relatively simple reagents under developed reaction condition. The promising biological activity of them and their expedient synthetic strategy were investigated. Furthermore, the obtained results were discussed, 132 novel compounds were synthesized and evaluated for in vitro cytotoxicity against four different tumor cells, in addition to their antioxidant activity. Also, they evaluated as photodynamic therapy. Structures of the newly synthesized compounds were inferred by computational chemistry, analytical and spectral data.