Provided herein are methods of isolating a 4-chloro-2-fluoro-3-substituted-phenylboronic acid. The method comprises contacting a mixture of water, a water-miscible organic solvent, and a 4-chloro-2-fluoro-3-substituted-phenylboronic acid with a salt to form a water-miscible organic solvent layer and a water layer. The 4-chloro-2-fluoro-3-substituted-phenylboronic acid is partitioned into the water-miscible organic solvent layer, which is separated from the water layer. Additional methods are disclosed, as is a 4-chloro-2-fluoro-3-substituted-phenylboronic acid produced by one of the methods, wherein the 4-chloro-2-fluoro-3-substituted-phenylboronic acid is obtained at a yield of greater than approximately 90%.