PURPOSE: To obtain the title compound useful as a phase transfer catalyst in organic reactions and separation or analysis simply in high yield on an industrial scale free from side reactions, by extracting a crown compound from its complex with a metal salt, using a specific solvent.

CONSTITUTION: A crown compound, e.g. crown ether, azacrown ether, or thiacrown ether, is extracted from its complex with a metal salt by means of a solvent consisting of an aliphatic hydrocarbon according to the liquid-solid or liquid-liquid extraction to give the desired crown compound. 4W8C Aliphatic hydrocarbons, e.g. butane, pentane, hexane, heptane or octane, or their mixture, may be cited as the solvent.