反应详情

A solution of bromine in 50 mL glacial acetic acid was added dropwise under nitrogen over 3 h to a solution of 2-ethyl-benzofuran-3-carboxylic acid (6-hydroxy-naphthalen-2-ylmethyl)-methyl-amide (1.5 g, 4.17 mmol), prepared in the previous step, in 150 mL glacial acetic acid at room temperature. The reaction stirred for 17 h (overnight). The solvent was removed under reduced pressure. The residue was dissolved in methylene chloride, extracted with 5% sodium bicarbonate, dried (MgSO4) and solvent removed under reduced pressure to give 2-ethyl-benzofuran-3-carboxylic acid (5-bromo-6-hydroxy-naphthalen-2-ylmethyl)-methyl-amide (1.74 g, 95%) as a brown solid, mp 176-178° C.

1. customThe solvent was removed under reduced pressure
2. dissolutionThe residue was dissolved in methylene chloride
3. extractionextracted with 5% sodium bicarbonate
4. dry with materialdried (MgSO4) and solvent
5. customremoved under reduced pressure