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
PROCEDURE
实验过程
A solution of sodium carbonate (0.31 g: 1.5 mmole) in 5 mL of water was added to a solution of N-(2-bromophenyl)-3-methylpyrazine-2-carboxamide (0.4 g: 1.4 mmole) and 4-trifluoromethoxyphenyl boric acid (0.31 g: 1.5 mmole) in 10 mL of toluene, followed by addition of tetrakis(triphenyl-Phosphine)palladium (0) (0.1 g: 0.09 mmole). After heating under reflux condition for 6 hours under argon atmosphere, the reaction mixture was cooled to room temperature, and admixed with ethyl acetate and water, followed by separation. The organic layer was washed with water and saturated brine successively, dried over anhydrous sodium sulfate, and concentrated in vacuo. The residue was purified by silica gel column chromatography to give the subject compound (0.35 g).
WORKUP
后处理
- temperatureAfter heating
- temperatureunder reflux condition for 6 hours under argon atmosphere
- customfollowed by separation
- washThe organic layer was washed with water and saturated brine successively
- dry with materialdried over anhydrous sodium sulfate
- concentrationconcentrated in vacuo
- customThe residue was purified by silica gel column chromatography