反应详情

To a stirred solution of 1-(5-chloro-2-hydroxy-4-methylphenyl)ethanone (20 g, 110 mmol) in acetic acid (200 mL) was added N-iodosuccinimide (29 g, 130 mmol) and the resulting mixture was stirred at room temperature for 18 hours. The reaction mixture was concentrated in vacuo, neutralized with saturated sodium bicarbonate, filtered off insoluble succinimide and extracted with ethyl acetate. The combined organic layers were washed with brine, dried over sodium sulfate, filtered and concentrated to dryness under reduced pressure. The crude product was recrystallized from a mixture of ethyl acetate and hexane (25.8 mg, 77%). LCMS calculated for C9H9ClIO2 (M+H)+: m/z=311.0. found: 311.0.

1. concentrationThe reaction mixture was concentrated in vacuo
2. filtrationfiltered off insoluble succinimide
3. extractionextracted with ethyl acetate
4. washThe combined organic layers were washed with brine
5. dry with materialdried over sodium sulfate
6. filtrationfiltered
7. concentrationconcentrated to dryness under reduced pressure
8. customThe crude product was recrystallized from a mixture of ethyl acetate and hexane (25.8 mg, 77%)