Conjugated linoleic acid (CLA) exhibits beneficial biological activities but possesses poor natural abundance, which is usually obtained by alkali isomerization of linoleic acid (LNA). The one‐pot alkali isomerization consists two reactions, firstly saponifying LNA and then isomerizing linoleate. This current process has been limited by two drawbacks, the overconsumption of both alkali and solvent, as well as the weak mass/heat transfer of the viscous paste of reaction mixture that limits the synthesis scale. The present study alternated the reaction pathway with a soap‐free preferential esterification pathway, that is, firstly employing slight NaOH to induce the esterification of LNA and diol (the reaction solvent), then conducting alkali isomerization of the intermediate alkyl linoleate instead of sodium linoleate. In this developed one‐pot procedure, a CLA yield of 90% and the selectivity of the desired isomers (“c9, t11” and “t10, c12” CLA) of 82.4% were obtained; and it reduced the consumption of NaOH and the solvent by 60% and 25% comparing to the current soap pathway, respectively; Yet the result is comparative to that obtained with assistant of microwave/ultrasound in even longer reaction time. In this way, the two drawbacks can be overcome and the green characteristics of the current process was well kept.
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