An efficient one-pot synthetic protocol for the synthesis of arylboronic esters has been established. The concentrated addition mixture of trimethylborate with aryl Grignard reagents was treated with low molecular weight diols (ethylene glycol, 1,3-propandiol) and toluene, the corresponding arylboronic esters were isolated in a convenient way with high yields. The diols not only serve as water replacement for the workup step, but also as well as the reagent for the preparation of arylboronic esters.