Methanol → Methyl 5-bromothiophene-2-carboxylate

Participants

Reaction Steps

Concentrated H2SO4 (3 mL) was added to a solution of 5-bromothiophene-2-carboxylic acid (5.0 g, 2.42 mmol) in methanol (100 mL). The reaction mixture was heated to reflux for 16 hours. After cooling to ambient temperature, the reaction mixture was concentrated to dryness. The residue was dissolved in EtOAc (60 mL), washed with saturated sodium carbonate (60 mL), and saturated sodium chloride (40 mL) and dried over anhydrous sodium sulfate. The solution was concentrated to give the compound 1021 (4.8 g). 1H NMR (CDCl3, 300 MHz) δ 3.90 (s, 3H), 7.09-7.10 (d, 1H), 7.57-7.58 (d, 1H).

Provenance & Evidence