反应详情

To a solution of 5.0 g of 4-(3,5-difluorophenoxy)phenol in 50 ml of carbon tetrachloride, there was added dropwise 2.45 g of t-butylhypochlorite with vigorously stirring and ice-cooling. After completion of the addition, the reaction mixture was stirred at room temperature for 5 hours and concentrated, followed by addition of 200 ml of ethyl acetate. The obtained solution was washed with an aqueous solution of 5% wt. sodium dicarbonate, dried and concentrated under reduced pressure. The residue was subjected to silica gel chromatography to give 5.31 g of 2-chloro-4-(3,5-difluorophenoxy)phenol. Yield. 92%. nD25 : 1.5639

1. temperatureice-cooling
2. additionAfter completion of the addition
3. stirringthe reaction mixture was stirred at room temperature for 5 hours
4. concentrationconcentrated
5. additionfollowed by addition of 200 ml of ethyl acetate
6. washThe obtained solution was washed with an aqueous solution of 5% wt. sodium dicarbonate
7. customdried
8. concentrationconcentrated under reduced pressure