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
To a stirred solution of 3,5-dibromo-4-chloropyridine (X, 0.5 g, 1.84 mmol) and cyclopropylboronic acid (0.17 g, 2.02 mmol), cesium carbonate (1.19 g, 3.68 mmol) in the mixture of 1,4-dioxan (10 mL) and water (2 mL). The reaction mass was purged with nitrogen for 15 min. Then catalyst Pd (dppf)2Cl2 (0.075 g, 0.09 mmol) was added and allowed to stir at 100° C. for 4 h. The reaction mixture was filtered through Mite bed and filter bed was thoroughly washed with ethyl acetate. The collected organic parts were concentrated under vacuum to afford the crude compound, which was purified by column chromatography using 10-40% ethyl acetate/hexane as an eluent to obtain title compound. MS (M+1): 233.0.
WORKUP
后处理
- customThe reaction mass was purged with nitrogen for 15 min
- filtrationThe reaction mixture was filtered through Mite bed
- filtrationfilter bed
- washwas thoroughly washed with ethyl acetate
- concentrationThe collected organic parts were concentrated under vacuum
- customto afford the crude compound, which
- customwas purified by column chromatography