反应详情

温度

100 °C

A solution of 3-bromoaniline (10.89 ml, TCI) in 20% aqueous hydrochloric acid (18.2 ml) was added with ammonium thiocyanate (8.02 g, WAKO) and sodium hydrogensulfite (701 mg, WAKO) and stirred at 100° C. for 22 hours. The reaction mixture was added with chloroform (20 ml) for extraction. The organic layer was dried, and then the solvent was evaporated under reduced pressure. The residue was purified by column chromatography (Quad, hexane:ethyl acetate=2:1) to obtain the title compound (Intermediate 62, 4.45 g).

1. customThe organic layer was dried
2. customthe solvent was evaporated under reduced pressure
3. customThe residue was purified by column chromatography (Quad, hexane:ethyl acetate=2:1)