The reaction of daunomycin (I) with trifluoroacetic anhydride in chloroform, and boiling the reaction product with methanol gives N-trifluoroacetyldaunomycin (II), which upon treatment with iodine and calcium oxide in THF gives 14-iodo-N-trifluoroacetyldaunomycin (III). Compound (III) treated with sodium valerate (A) in boiling acetone gives the title compound. The final purification is achieved with silicic acid using chloroform-ethanol (100:1) as solvent.