To obtain an alkylimide ether sulfate with industrial advantage by allowing an aliphatic nitrile and an alcohol to react with sulfuric acid under mild reaction conditions with reduced corrosion of installation, for example, reactor or the like.

An aliphatic nitrile (for example, valeronitrile) and an alcohol (for example, methanol) are allowed to react with sulfuric acid. In an embodiment, the aliphatic nitrile is mixed with an alcohol, then sulfuric acid is admixed at a reaction temperature of 0-15°C, preferably 5-10°C. Then, the reaction mixture is kept at 0-20°C, preferably 8-15°C in the reaction mixture under stirring for 1-20 hours, particularly for 5-15 hours for aging. In a preferred embodiment, the amount of the alcohol to be used in the reaction is ≥1 mole, particularly 1.0-1.5 mole per mole of the aliphatic nitrile. The amount of the sulfuric acid is preferably ≥0.5 mole, particularly 0.6-0.8 mole per mole of the nitrile.