An unusual synthesis of porphyrin has been developed using a novel biphasic solvent system. Under optimized conditions reproducible yields of pure porphyrin of over 15% can be easily obtained in about two hours from the acid-catalysed condensation of 2-hydroxymethylpyrrole in a solvent consisting of water and an immiscible ketone. Important variables of the reaction have been studied to improve the yield and characterize the limitations of the reaction.