反应详情

Under heating, a 1-propanol (50 ml) solution of 4-chloromethylpyridine hydrochloride (1.26 g, 7.65 mmol), sodium 4-chlorobenzenesulfinate (1.52 g, 7.65 mmol) and potassium acetate (1.50 g, 15.3 mmol) was stirred at 70° C. for 8 hours. After cooling to room temperature, the reaction mixture was concentrated under reduced pressure. The residue was filtered through a short column (silica gel, ethyl acetate) and the eluate was concentrated under reduced pressure. The residue was subjected to chromatography on a silica gel column, and the fraction obtained from the hexane:ethyl acetate (=2:3) eluate was concentrated under reduced pressure, whereby the title compound (1.26 g, 62%) was obtained as a white solid.

1. temperatureUnder heating
2. concentrationthe reaction mixture was concentrated under reduced pressure
3. filtrationThe residue was filtered through a short column (silica gel, ethyl acetate)
4. concentrationthe eluate was concentrated under reduced pressure
5. customthe fraction obtained from the hexane
6. concentrationethyl acetate (=2:3) eluate was concentrated under reduced pressure, whereby the title compound (1.26 g, 62%)
7. customwas obtained as a white solid