反应详情

Nitric acid (40 ml, excess) was added drop wise over 20 minutes to a stirred solution of 5-methyl-1H-benzotriazole (2.66 g, 20 mmol) in conc. sulphuric acid (40 ml) at 0° C. Stirring was continued at room temperature for 90 minutes by which time TLC (A) indicated complete reaction. The solution was poured onto ice to precipitate a flocculent white solid. The solid was collected by filtration and washed with water to afford [23] in 94% yield. Rf (A) 0.60 δH(400 MHz; DMSO-d6) 2.79 (3H, s, CH3) 7.52 (1H, d, J8.4, BT) 8.36 (1H, br s, BT) 16.26 (1H, s, NH); m/z (EI−HR) 178.04937 [(M) calc. for C7H6N4O2 178.04908].

1. customreaction
2. additionThe solution was poured onto ice
3. customto precipitate a flocculent white solid
4. filtrationThe solid was collected by filtration
5. washwashed with water