反应详情

50 ml (0.56 mole) of methyl disulfide in 400 ml of 2.4-lutidine was added 46 g (0.72 mole) of copper. The mixture was heated at 140° for 3 hours. The solution was cooled to room temperature and 74.90 g (0.56 mole) of 3-bromo-5-methoxy-4-propoxybenzaldehyde was then added. The mixture was refluxed for 16 hours at 175° C. The solution was filtered and the filtrate was concentrated to dryness. The product was purified by flash column chromatography first then recrystallized from hexane to give 17.01 g (26% yield) of 3-methoxy-5-methylthio-4-propoxybenzaldehyde as a white solid. m.p. 64°-66° C.

1. temperatureThe mixture was heated at 140° for 3 hours
2. temperatureThe mixture was refluxed for 16 hours at 175° C
3. filtrationThe solution was filtered
4. concentrationthe filtrate was concentrated to dryness
5. customThe product was purified by flash column chromatography first
6. customrecrystallized from hexane