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A process for the preparation of iodixanol by dimerisation of 5-acetamido-N, N′-bis (2, 3-dihydroxypropyl)-2, 4, 6-triiodo-isophthalamide (“Compound A”) in which, after the dimerisation step, unreacted Compound A is precipitated from the reaction mixture and recovered for re-use. The process substantially increases the net yield of iodixanol and simplifies its purification.