The pyrogallolarene macrocycle is typically prepared by condensation of pyrogallol and an aldehyde in concentrated acid solution in the presence of an alcohol solvent, usually methanol or ethanol. The reaction conditions can usually be carefully adjusted to precipitate the pure product or the product may be purified by recrystallization.
Pyrogallol[4]arene is simply made by mixing a solvent-free dispersion of isovaleraldehyde with pyrogallol, and a catalytic amount of p-toluenesulfonic acid, in a mortar and pestle.