HRID535384
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
- 90 °C
PROCEDURE
实验过程
A mixture of 6-chloro-4-(trifluoromethyl)pyridin-2-amine (1.0 g, 5.09 mmol) ethynylbenzene (779 mg, 7.63 mmol), 1,1′-Bis(diphenylphosphino)ferrocene]dichloro-palladium(II) (372 mg, 0.51 mmol), copper(I) iodide (96 mg, 0.51 mmol), triethylamine (1.8 ml, 12.7 mmol), ACN (10 ml) and THF (5 ml) is stirred for 6 h at 90° C. The mixture is concentrated in vacuo, water is added (100 ml) and the mixture extracted with EtOAc. The combined organic layers are dried over MgSO4 and concentrated in vacuo. The product is purified by NP chromatography. Yield: 680 mg (51%). HPLC-MS: M+H=263.
WORKUP
后处理
- concentrationThe mixture is concentrated in vacuo, water
- additionis added (100 ml)
- extractionthe mixture extracted with EtOAc
- dry with materialThe combined organic layers are dried over MgSO4
- concentrationconcentrated in vacuo
- customThe product is purified by NP chromatography