反应详情

Sodium hydride (60% dispersion in oil, 15 mg, 0.38 mmol) was added to tetrahydrofuran (10 ml). Under ice cooling, the 2-[(4-chlorophenyl)sulfonylmethyl]-1,4-difluorobenzene (100 mg, 0.330 mmol) obtained in Example 5 was added. After stirring the reaction mixture at room temperature for 30 minutes, 1,5-dibromopentane (0.10 ml, 0.74 mmol) was added. The reaction mixture was stirred at room temperature for 3 days, followed by the addition of sodium hydride (60% dispersion in oil, 15 mg, 0.38 mmol) under ice cooling. The resulting mixture was stirred at room temperature for 15 minutes and then added with 1,5-dibromopentane (0.10 ml, 0.74 mmol). The mixture was stirred at room temperature for 14 hours and then concentrated under reduced pressure. The residue thus obtained was purified by silica gel chromatography (hexane:ethyl acetate=10:1) to yield a white solid. The resulting white solid was washed with hexane, whereby the title compound (51 mg, 30%) was obtained as a white powder.

1. stirringThe reaction mixture was stirred at room temperature for 3 days
2. stirringThe resulting mixture was stirred at room temperature for 15 minutes
3. stirringThe mixture was stirred at room temperature for 14 hours
4. concentrationconcentrated under reduced pressure
5. customThe residue thus obtained
6. customwas purified by silica gel chromatography (hexane:ethyl acetate=10:1)
7. customto yield a white solid
8. washThe resulting white solid was washed with hexane, whereby the title compound (51 mg, 30%)
9. customwas obtained as a white powder