618-51-9

25487-66-5

618-51-9

The general procedure for the synthesis of 3-iodobenzoic acid from 3-carboxyphenylboronic acid was as follows: arylboronic acid 1 (0.5 mmol) and K2CO3 (1 mmol, 138.0 mg) were added to a 20 mL Schlenk tube fitted with a non-magnetic stir bar. The Schlenk tube was evacuated twice and backfilled with N2. MeCN (2 mL) and I2 (0.75 mmol, 191 mg) were added to the tube at room temperature. The Schlenk tube was sealed and placed in a preheated oil bath at 80 °C for 8-12 h under a stream of N2 gas. After completion of the reaction, the resulting solution was cooled to room temperature. H2O (10 mL) was added, and for the product 3-iodobenzoic acid, 1 M HCl was added to the aqueous solution until the pH reached 2 prior to extraction.The aqueous layer was extracted with EtOAc (3 x 5 mL). The organic phases were combined, dried with anhydrous Na2SO4, filtered and concentrated by rotary evaporation. Finally, the residue was purified by silica gel column chromatography to obtain the target product 3-iodobenzoic acid.