反应详情

温度

30 °C

6-Cyclopropyl-2,4-dihydroxy-pyridine (1 g, 6.6 mmol) was suspended in AcOH:EtOAc (4:1, 10 mL) at room temperature. The mixture was warmed to 30° C. and a small portion of fuming nitric acid (0.05 ml, 1.2 mmol) was added dropwise, keeping the temperature between 30 and 35° C. Upon addition the mixture became a clear solution. The remainder of the fuming nitric acid (0.25 ml, 6.3 mmol) was added dropwise. The clear solution was allowed to cool to room temperature upon which a precipitate started to form. The mixture was stirred at room temperature overnight. The solid was collected by filtration, washed with cold water and Et2O and dried in vacuo at room temperature over the weekend to give the title compound (1.21 g) as a yellow powder.

1. customthe temperature between 30 and 35° C
2. additionUpon addition the mixture
3. temperatureto cool to room temperature upon which a precipitate
4. customto form
5. filtrationThe solid was collected by filtration
6. washwashed with cold water and Et2O
7. customdried in vacuo at room temperature over the weekend