反应详情

A mixture of 0.50 g (1.28 mmol) of 4-(4-methylsulfonylaminophenylthio)-1-[2-(3-pyridyl)-ethyl]piperidine, 0.33 g (1.53 mmol) of sodium periodate, 5 ml of 1 N hydrochloric acid and 5 ml of methanol was stirred at room temperature for 1 h. About 5 ml of a 1 N sodium hydroxide solution was added thereto to adjust the pH to about 7. After extraction with chloroform, the organic layer was concentrated and the residue was purified by silica gel column chromatography (CHCl3 :CH3OH: NH4OH=95:5:0.5). The fraction containing the intended compound was concentrated to give a solid residue, which was recrystallized from ethyl acetate to give a 0.34 g (yield: 64%) of the compound.

1. extractionAfter extraction with chloroform
2. concentrationthe organic layer was concentrated
3. customthe residue was purified by silica gel column chromatography (CHCl3 :CH3OH: NH4OH=95:5:0.5)
4. additionThe fraction containing the intended compound
5. concentrationwas concentrated
6. customto give a solid residue, which
7. customwas recrystallized from ethyl acetate