反应详情

6.0 mL nitric acid were added dropwise to 6.0 mL conc. sulphuric acid while cooling with ice and stirring. Then 3.6 g (21 mmol) 5-bromo-2-methylpyridine-1-oxide were added batchwise and the reaction mixture was stirred for 18 h at 60° C. After cooling to RT the reaction mixture was added to ice water and neutralised with 4N aqueous sodium hydroxide solution. The precipitated solid was suction filtered and dried at 50° C.

1. temperaturewhile cooling with ice
2. stirringthe reaction mixture was stirred for 18 h at 60° C
3. filtrationfiltered
4. customdried at 50° C.