反应详情

The 2-[(4-chlorophenyl)sulfonylmethyl]-1,4-difluorobenzene (0.94 g, 3.1 mmol) obtained in Example 5 was dissolved in toluene (15 ml). After addition of 4-(methylthio)-1-butanol (0.25 ml, 2.1 mmol) and cyanomethylenetri-n-butylphosphorane (1.0 g, 4.1 mmol), the resulting mixture was heated under reflux for 14 hours under an argon atmosphere. The reaction mixture was allowed to cool down. Then, 4-(methylthio)-1-butanol (0.25 ml, 2.1 mmol) was added, followed by heating under reflux for 6 hours under an argon atmosphere. The reaction mixture was allowed to cool down and then, concentrated under reduced pressure. The residue thus obtained was purified by silica gel chromatography (hexane:ethyl acetate=10:1) to yield a colorless oil. The resulting colorless oil was solidified with hexane, whereby the title compound (0.55 g, 44%) was obtained as a white powder.

1. temperaturethe resulting mixture was heated
2. temperatureunder reflux for 14 hours under an argon atmosphere
3. temperatureto cool down
4. temperatureby heating
5. temperatureunder reflux for 6 hours under an argon atmosphere
6. temperatureto cool down
7. concentrationconcentrated under reduced pressure
8. customThe residue thus obtained
9. customwas purified by silica gel chromatography (hexane:ethyl acetate=10:1)
10. customto yield a colorless oil