反应详情

温度

150 °C

To 4-chloro-6-methylpyridin-2-amine (100 mg, 0.701 mmol) and 1,2,3-triazole (0.133 mL, 2.30 mmol) in a pressure tube was added DIPEA (0.185 mL, 1.06 mmol). The reaction mixture was sealed and heated at 150° C. for 1.5 hours. The reaction mixture was cooled, diluted with DCM (20 mL), and washed with water (10 mL). The organics were separated, dried over sodium sulfate, filtered, and concentrated under reduced pressure. The residue was slurried in 5% methanol/ethyl acetate (5 mL) and sonicated. The mixture was filtered, and the collected solids were dried under reduced pressure to afford 6-methyl-4-(1H-1,2,3-triazol-1-yl)pyridin-2-amine. MS ESI calc'd. for C8H10N5 [M+H]+ 176. found 176. 1H NMR (500 MHz, DMSO-d6) δ 8.79 (s, 1H), 7.95 (s, 1H), 6.90 (s, 1H), 6.75 (s, 1H), 6.28 (s, 2H), 2.23 (s, 3H).

1. customThe reaction mixture was sealed
2. temperatureThe reaction mixture was cooled
3. washwashed with water (10 mL)
4. customThe organics were separated
5. dry with materialdried over sodium sulfate
6. filtrationfiltered
7. concentrationconcentrated under reduced pressure
8. customsonicated
9. filtrationThe mixture was filtered
10. customthe collected solids were dried under reduced pressure