HRID1045811
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 150 °C
PROCEDURE
实验过程
2,6-Dichloropyrazine (1.0 g, 6.7 mmol, 1.0 eq), 3-hydroxypyridine (638 mg, 6.71 mmol, 1.00 eq) and K2CO3 (1.11 g, 8.03 mmol, 1.20 eq) were dissolved in DMF (10 mL) and heated in a microwave for 15 minutes at 150° C. The reaction was cooled, diluted with EtOAc and washed with H2O (3×). The organic layer was dried (MgSO4), filtered and concentrated in vacuo. Purification by flash chromatography on silica gel afforded 1.3 g (93%) of the title compound as a white solid: 1H NMR (400 MHz, CDCl3) δ 8.59 (d, J=2.3 Hz, 1H), 8.56 (d, J=4.4 Hz, 1H), 8.41 (s, 1H), 8.37 (s, 1H), 7.71 (dq, J=8.4, 1.3 Hz, 1H), 7.51 (dd, J=8.4, 4.9 Hz, 1H); ES-MS [M+1]+: 208.1.
WORKUP
后处理
- temperatureThe reaction was cooled
- washwashed with H2O (3×)
- dry with materialThe organic layer was dried (MgSO4)
- filtrationfiltered
- concentrationconcentrated in vacuo
- customPurification by flash chromatography on silica gel