反应详情

温度

50 °C

To a solution of 5-(4-chlorophenyl)-2-furoic acid (5.0 g, 22 mmol) in MeOH (50 mL) was added conc. H2SO4 (4 drops) and the resulting solution heated to 50° C. for 4 days. The reaction was cooloed and concentrated in vacuo. The residue was taken up in EtOAc (100 mL) and washed with saturated aqueous NaHCO3 (2×20 mL), dried (MgSO4) and concentrated in vacuo. The residue was purified by flash cjromatography (hexane/EtOAc 19:1) to give 3.8 g (72%) of a cream powder; MS m/z 254 (M++18, 100).

1. concentrationconcentrated in vacuo
2. washwashed with saturated aqueous NaHCO3 (2×20 mL)
3. dry with materialdried (MgSO4)
4. concentrationconcentrated in vacuo
5. customThe residue was purified by flash cjromatography (hexane/EtOAc 19:1)