HRID923659
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
- 50 °C
PROCEDURE
实验过程
Under argon atmosphere dichlorobis(triphenylphosphine)palladium(II) (1.6 g, 2.2 mmol) is added to a mixture of 2-amino-4,6-dibromopyridine (5.44 g, 21.6 mmol), ethynyl-tri(propan-2-yl)silane (5.1 g, 28.1 mmol), copper(I) iodide (0.44 g, 2.3 mmol) and triethylamine (9 ml, 64 mmol) in ACN (32 ml) with THF (16 ml). After stirring at 50° C. for 17 h the mixture is diluted with water and extracted with EtOAc. The combined organic layers are dried over MgSO4 and concentrated in vacuo. The product is purified by NP chromatography. Yield: 4.7 g (62%). HPLC-MS: M+H=353/355; tR=1.80 min (METHOD—1).
WORKUP
后处理
- extractionextracted with EtOAc
- dry with materialThe combined organic layers are dried over MgSO4
- concentrationconcentrated in vacuo
- customThe product is purified by NP chromatography