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Alkyl nitrites were prepared in good to excellent yields by treatment of alcohols, thiols and trimethylsilyl ethers with 2,4,6-trichloro[1,3,5]triazine/n-Bu4NNO2 in refluxing acetonitrile. This method is highly selective for the conversion of primary alcohols to alkyl nitrites in the presence of secondary and tertiary alcohols, thiols and trimethylsilyl ethers.