反应详情

温度

60 °C

Sodium nitrite (0.708 g, 10.25 mmol) was added to a mixture of 5-iodo-3-methyl-pyridin-2-ylamine (2 g, 8.55 mmol) and H2SO4 (12 mL) at 0° C. The reaction mixture was stirred 15 min at 60° C., allowed to cool down, and poured onto crushed ice. Boric acid (1.057 g, 17.09 mmol) was added and the solution was quickly heated to 100° C. The reaction mixture was cooled down and neutralized with a saturated aq. NH4OH solution. The suspension was filtered to afford the crude title product (1.67 g, 7.11 mmol, 83% yield) as a brown solid. tR: 2.85 min (HPLC 1); tR: 0.62 min (LC-MS 2); ESI-MS: 236 [M+H]+ (LC-MS 2).

1. temperatureto cool down
2. additionpoured
3. customonto crushed ice
4. temperaturethe solution was quickly heated to 100° C
5. temperatureThe reaction mixture was cooled down
6. filtrationThe suspension was filtered