反应详情

To an ice cold (−10° C.) solution of concentrated sulfuric acid (5 mL) was added 3-methylthiopheno[2,3-d]1,2,3-triazin-4-one (0.6 g, 3.6 mmol) for 10 min., nitric acid (0.4 mL, 9 mmol) was added to the above reaction mixture for 5 min and the mixture was attained to rt and stirred for 1 h. The mixture was poured into ice cold water and stirred for 15 min. The precipitated solid was filtered and purified by silica gel column chromatography using hexane-chloroform (1:1) as eluents to give the product as a pale yellow color solid (390 mg, 51%), mp 164-168° C. 1H NMR (400 MHz, DMSO-d6): δ 8.60 (1H, s), 3.99 (3H, s).

1. customwas attained to rt
2. additionThe mixture was poured into ice cold water
3. stirringstirred for 15 min
4. filtrationThe precipitated solid was filtered
5. custompurified by silica gel column chromatography