反应详情

A solution of 4,6-dichloro-5-pyrimidinecarbaldehyde (15.0 g, 84.8 mmol) in DMF (360 mL) was charged with potassium monopersulfate (38.9 g, 254 mmol) and stirred over night at rt. The reaction mixture was filtered through a pad of celite and partitioned between EtOAc and water and separated. The aqueous was extracted with EtOAc (3×) and the combined organic fractions were washed with water (2×), brine, and dried over sodium sulfate, filtered, and concentrated to afford the title compound. 1H NMR (DMSO-d6, 400 MHz): δ=9.02 (s, 1H).

1. filtrationThe reaction mixture was filtered through a pad of celite
2. custompartitioned between EtOAc and water
3. customseparated
4. extractionThe aqueous was extracted with EtOAc (3×)
5. washthe combined organic fractions were washed with water (2×), brine
6. dry with materialdried over sodium sulfate
7. filtrationfiltered
8. concentrationconcentrated