反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 100 °C
PROCEDURE
实验过程
A mixture of crude 8-bromo-1-methyl-[1,2,4]triazolo[4,3-a]quinoxaline (809 mg, 3.07 mmol), PdCl2(dppf)2 (132.6 mg, 0.153 mmol), 2-methoxy-5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyridin-3-amine (1 g, 4.3 mmol) and K2CO3 (1.7 g, 12.28 mmol) in DMF (40 mL) and water (15 mL) was stirred at 100° C. overnight. Half of solvent was removed. After cooling to room temperature, the resulting mixture was poured into ice-water. The precipitate was collected, washed with water three times, and dried in vacuo to afford crude 2-methoxy-5-(1-methyl-[1,2,4]triazolo[4,3-a]quinoxalin-8-yl)pyridin-3-amine as grey solid (730 mg, yield 77%) which was used in next step without further purification. MS (m/z): 307 (M+H)+.
WORKUP
后处理
- customHalf of solvent was removed
- temperatureAfter cooling to room temperature
- additionthe resulting mixture was poured into ice-water
- customThe precipitate was collected
- washwashed with water three times
- customdried in vacuo