反应详情

温度

70 °C

To dimethoxyethane (10 ml) were added sodium 4-chlorobenzenesulfinate (205 mg, 1.03 mmol) and 2,6-difluorobenzyl bromide (214 mg, 1.03 mmol). The resulting mixture was stirred at 70° C. for 18 hours. After cooling the reaction mixture to room temperature, the solvent was concentrated under reduced pressure. Ethyl acetate was added to the residue and from the resulting mixture, the insoluble matter was filtered off. The filtrate was concentrated under reduced pressure. The residue was subjected to chromatography on a silica gel column and the fraction obtained from the ether eluate was concentrated under reduced pressure. The residue was subjected to chromatography on a silica gel column. The fraction obtained from the hexane:ethyl acetate (=10:1) eluate was concentrated under reduced pressure, whereby the title compound (289 mg, 93%) was obtained as a white solid.

1. temperatureAfter cooling the reaction mixture to room temperature
2. concentrationthe solvent was concentrated under reduced pressure
3. additionEthyl acetate was added to the residue and from the resulting mixture
4. filtrationthe insoluble matter was filtered off
5. concentrationThe filtrate was concentrated under reduced pressure
6. customthe fraction obtained from the ether eluate
7. concentrationwas concentrated under reduced pressure
8. customThe fraction obtained from the hexane
9. concentrationethyl acetate (=10:1) eluate was concentrated under reduced pressure, whereby the title compound (289 mg, 93%)
10. customwas obtained as a white solid