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Diesters are important synthetic tools for many biologically active compounds. There are only few methods known for the synthesis of diesters, however the known methods have their own limitations such as substrate scope and drastic reactions conditions. Carbonylation of diazo compounds using Co2(CO)8 as a carbonyl source and generating ketene finds many useful applications in synthetic chemistry. In this regard, we have utilized the methodology to synthesize diesters via nucleophilic addition of alcohol to the ketene generated from diazo compounds using Co2(CO)8 as a carbonyl source and catalyst, under mild reaction conditions. Both aliphatic and aromatic alcohols with electron withdrawing and donating substituents are well tolerated giving rise to a large number of biologically active diesters in good yield, which is further characterized by standard analytical and spectroscopic techniques. [ABSTRACT FROM AUTHOR]