反应详情

温度

70 °C

A mixture of 2-chloro-N-(4-fluoro-2-phenylaminophenyl)acetamide (740 mg, 2.62 mmol) in AcOH (20 mL) was heated at 70° C. for 5 h under a nitrogen atmosphere. The volatiles were removed in vacuo and the resulting residue partitioned between DCM and a saturated aqueous solution of NaHCO3. The aqueous phase was further extracted with DCM (×3) and the combined organic fractions washed with water, dried (Na2SO4) and concentrated in vacuo. The resulting residue was purified by column chromatography (Si—PCC, gradient 0-5% MeOH in DCM) to afford the title compound as a brown oil which crystallised on standing (570 mg, 84%). LCMS (Method C): RT 3.40 min [M+H]+ 261.2.

1. customThe volatiles were removed in vacuo
2. customthe resulting residue partitioned between DCM
3. extractionThe aqueous phase was further extracted with DCM (×3)
4. washthe combined organic fractions washed with water
5. dry with materialdried (Na2SO4)
6. concentrationconcentrated in vacuo
7. customThe resulting residue was purified by column chromatography (Si—PCC, gradient 0-5% MeOH in DCM)