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This paper reports the results of an FT-IR and NIR study of N-methylformamide in carbon tetrachloride solution in presence of ethers as the O--electron donors, i.e., diethyl ether (DEE), diisopropyl ether (DiPE), methyl t--butyl ether (MtBE), dibutyl ether (DBE), dipentyl ether (DPE), tetrahydro-furan (THF) and tetrahydropyran (THP). The spectroscopic characteristics of the N–H•••O hydrogen bonded complexes are given. In addition, the equilibrium constants for 1:1 complex formation were determined at 25 °C using Mid-IR and NIR measurements.