反应详情

Process 3: After addition of 2-bromomethyl-1,4-difluorobenzene (12.3 ml, 95.5 mmol) to a suspension of sodium 4-chlorobenzenesulfinate (19.0 g, 95.5 mmol) in butanol (200 ml), the mixture was heated under reflux for 5 hours. The solid thus precipitated was collected by filtration and dissolved in methylene chloride. The resulting solution was washed with brine, dried over MgSO4, and concentrated. The solid thus obtained was recrystallized from hexane, whereby the title compound (12.3 g, 43%) was obtained as colorless needle crystals.

1. temperaturethe mixture was heated
2. temperatureunder reflux for 5 hours
3. customThe solid thus precipitated
4. filtrationwas collected by filtration
5. dissolutiondissolved in methylene chloride
6. washThe resulting solution was washed with brine
7. dry with materialdried over MgSO4
8. concentrationconcentrated
9. customThe solid thus obtained
10. customwas recrystallized from hexane, whereby the title compound (12.3 g, 43%)
11. customwas obtained as colorless needle crystals