IBX can be prepared in a single step by adding an excess of oxone to an aqueous solution of 2-iodobenzoic acid.

After warming the solution to 70°C for three hours, the precipitated IBX is collected as a white crystalline solid (80% yield, ≥95% purity).

Purity can be increased (≥99%) by shorting the reaction time to one hour at 70°C, at the cost of slightly reducing yield to 77%.

The twist is a requirement because the iodine to oxygen double bond is oriented out of plane with the alkoxy group and the concerted elimination would not be able to take place.

In 2001, K. C. Nicolaou and co-workers published a series of papers in the Journal of the American Chemical Society demonstrating, among other transformations, the use of IBX to oxidize primary and secondary benzylic carbons to aromatic aldehydes and ketones, respectively.

[12] This method could be extended to β-keto esters,[13] and forms a regioselective way to introduce conjugatively activated unsaturation.