反应详情

To a solution of (4-bromo-phenyl)-acetic acid ethyl ester (972.4 mg, 4 mmol), paraformaldehyde (240 mg, 8 mmol), and Bu4NCl (22 mg, 0.08 mmol) in DMF (10 mL) was added K2CO3 (1.32 g, 9.6 mmol). This mixture was heated at 60 degrees Celsius for 2 h. Then the mixture was cooled and diluted with EtOAc (30 mL) and washed with water (20 mL×3), brine, dried over Na2SO4, filtered and evaporated. The residue was purified by flash column chromatography on silica gel to give a white solid (0.74 g, 73%). MS: calc'd 255 (MH+), exp 255 (MH+).

1. temperatureThis mixture was heated at 60 degrees Celsius for 2 h
2. temperatureThen the mixture was cooled
3. washwashed with water (20 mL×3), brine
4. dry with materialdried over Na2SO4
5. filtrationfiltered
6. customevaporated
7. customThe residue was purified by flash column chromatography on silica gel