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Disclosed is a process for the preparation of a compound of general formula (III), which comprises the reaction between a compound of general formula (V) and dicyano acetylene (IV), said reaction carried out in the presence of water (see formula IV) (see formula V) (see formula III) wherein R is selected from the group consisting of CF3, and C1 to C6 alkyl; and M is an alkaline or alkaline-earth metal or silver. The compound of general formula (III) may be used in the synthesis of pesticidally active compounds such as fipronil.