反应详情

温度

60 °C

A solution 1-methylisoquinoline (D91) (1 g, 7 mmol) in sulfuric acid (2.5 ml) was cooled (<4° C.) and concentrated nitric acid (1 ml) was added over 10 mins. The reaction was stirred for 30 mins and then heated at 60° C. for 2 h. After cooling, the reaction mixture was poured into ice water slurry (100 ml) and basified using solid potassium carbonate followed by extraction with DCM. The organic phase was separated, dried over MgSO4, filtered and concentrated in vacuo to afford the product as a white solid (1.05 g). 1H NMR (400 MHz, DMSO) δ (ppm): 8.69 (d, 1H), 8.59 (m, 2H), 8.11 (d, 1H), 7.88 (t, 1H), 2.99 (s, 3H).

1. additionwas added over 10 mins
2. temperatureAfter cooling
3. extractionfollowed by extraction with DCM
4. customThe organic phase was separated
5. dry with materialdried over MgSO4
6. filtrationfiltered
7. concentrationconcentrated in vacuo