反应详情

温度

60 °C

A solution of 5-amino-6-methylpicolinonitrile (2) (260 mg, 1.95 mmol), CuCl (290 mg, 2.93 mmol) and t-BuONO (456 mg, 3.9 mmol) in CH3CN (10 mL) was stirred at room temperature under N2 for 2 h, and then warmed to 60° C. After 2 h, 10 mL 6N HCl was added and extracted with EA (3×10 mL). The organic phase was dried with anhydrous Na2SO4, filtered and concentrated. The residue was purified by Prep-TLC using PE/EtOAc=1/1 to give title compound as oil.

1. extractionextracted with EA (3×10 mL)
2. dry with materialThe organic phase was dried with anhydrous Na2SO4
3. filtrationfiltered
4. concentrationconcentrated
5. customThe residue was purified by Prep-TLC