反应详情

To a mixture of 2-[4-(3,5-difluorophenoxy)phenoxy]ethanol (1.00 g, 3.76 mmol) and n-hexane (50 ml), phosphorus tribromide (0.71 g, 2.63 mmol) was gradually added with stirring under ice-cooling. After completion of the addition, the temperature was elevated to room temperature and stirring was continued at the same temperature for 30 minutes, followed by stirring under reflux for 1 hour. After allowed to cool, the upper n-hexane layer was collected by decantation, and the n-hexane layer was washed with water two times, an aqueous sodium carbonate solution three times and a saturated aqueous sodium chloride solution once in order and dried over anhydrous magnesium sulfate. Removal of the solvent gave 2-[4-(3,5-difluorophenoxy)phenoxy]ethyl bromide (915 mg).

1. additionwas gradually added
2. temperaturecooling
3. additionAfter completion of the addition
4. customwas elevated to room temperature
5. stirringstirring
6. stirringby stirring
7. temperatureunder reflux for 1 hour
8. temperatureto cool
9. customthe upper n-hexane layer was collected by decantation
10. washthe n-hexane layer was washed with water two times
11. dry with materialan aqueous sodium carbonate solution three times and a saturated aqueous sodium chloride solution once in order and dried over anhydrous magnesium sulfate
12. customRemoval of the solvent