反应详情

To a solution of 3,4-difluorophenol (1.56 g, 7.69 mmol) in dichloromethane (10 mL) under a blanket of nitrogen is added ammonium nickel sulfate (2.0 g, 5.07 mmol), with vigorous stirring, followed by the addition of nitric acid (69%, 0.770 mL, 7.69 mmol). The resulting heterogeneous mixture is then stirred at RT for 5-10 min; at this point a bright orange solution was observed along with a mild exothermic gaseous emission. (LC/MS indicated the formation of one single product.) Anhydrous magnesium sulfate (˜1 g) is then added to the reaction mixture, which is stirred and filtered to afford an orange solution. Removal of dichloromethane under reduced pressure affords an orange solid residue. (low melting solid, sublimed upon storage) 1H NMR (400 MHz, δ, CDCl3): 10.61 (s, 1H), 8.01 (m, 1H), 7.00 (m, 1H).

1. stirringis stirred
2. filtrationfiltered
3. customto afford an orange solution
4. customRemoval of dichloromethane under reduced pressure
5. customaffords an orange solid residue