This invention belongs to the technical field of
organic synthesis and discloses a method for preparing benzo[i]iodo[i]oxapentane
reagent. The method involves adding
periodic acid or
periodate as an oxidant, along with an o-iodobenzyl
alcohol compound, to an aqueous
acetic acid solution. Heating causes a
redox reaction, followed by recrystallization or slurrying to obtain the product, benzo[i]iodo[i]oxapentane
reagent. R1 is selected from methyl or
trifluoromethyl; R2 is selected from
hydrogen,
halogen, or methyl; R3 is selected from
hydrogen or methyl; and
periodate is selected from
sodium periodate,
potassium periodate, tetrabutylammonium
potassium periodate, or
lithium periodate. This invention provides a one-step, efficient method for preparing benzo[i]iodo[i]oxapentane
reagent using
periodic acid / salt, with simple steps and easily separable reaction products. The
redox reaction equation is as follows: