A process for the recovery of a Lewis acid from a reaction mixture (I) which has been obtained in the hydrocyanation of an olefinically unsaturated compound to a nitrile which has a miscibility gap with water under certain pressure and temperature conditions, in the presence of a catalyst system comprising a Lewis acid and a complex compound. The method comprises a) removing the complex compound from mixture (I) to give a mixture (II), b) adding water to mixture (II) and placing mixture (II) under pressure and temperature conditions to provide a phase (III) and a phase (IV), c) adding a liquid diluent (V) which c1) does not form an azeotrope with water and whose boiling point under certain pressure conditions is higher than that of water, or c2) forms an azeotrope or heteroazeotrope with water under certain pressure conditions,  to phase (III), d) subjecting the mixture of phase (III) and liquid diluent (V) to distillation under the pressure conditions mentioned in step c1) or c2), and e) subjecting mixture (VII) to hydrocyanation of an olefinically unsaturated compound to give the nitrile