3,4-Difluoro-1,2-benzenedicarboxylic acid → HCID 59314172, compound

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Reaction Steps

To a suspension of LAH (6.2 g, 0.163 mol) in dry THF (100 ml) is added a solution of compound 3,4-difluoro-phthalic acid (15 g, 0.074 mol) in THF (75 mL), drop wise at 0° C. The resulting mixture is refluxed for 3 h. After 3 h the reaction mixture is cooled and quenched with saturated Na2SO4 solution. Then the reaction mass is filtered through a pad of celite and the bed is washed thoroughly with MeOH. The combined filtrate is concentrated to yield a crude product that is purified by column chromatography (silica, 5% MeOH in DCM). Combination of appropriate fractions followed by removal of the solvent yields white solid (7 g, 54.2%).

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