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 round-bottomed flask equipped with a stirring bar, 138b (2.52 g, 12.22 mmol), 3,5-dibromo-1-methylpyridin-2(1H)-one (4.89 g, 18.32 mmol), Pd2(dba)3 (1.12 g, 1.22 mmol), XantPhos (1.13 mg, 1.96 mmol), Cs2CO3 (13.14 g, 40.33 mmol) and dioxane (50 mL) were added. The reaction mixture was heated at 100° C. overnight. CH2Cl2 (200 mL) was added to the resulting mixture was washed with water (30 mL×3). CH2Cl2 (200 mL) was added and the resulting mixture was washed with water (30 mL×3), brine (30 mL×1), dried over MgSO4, filtered, and removed solvent in vacuo. CH2Cl2/ether (1:2, 5 mL) was added followed by sonication, the precipitation was filtered as 138c, a yellow solid, 2.718 g (57%).
WORKUP
后处理
- customTo a round-bottomed flask equipped with a stirring bar
- washwas washed with water (30 mL×3)
- additionCH2Cl2 (200 mL) was added
- washthe resulting mixture was washed with water (30 mL×3), brine (30 mL×1)
- dry with materialdried over MgSO4
- filtrationfiltered
- customremoved solvent in vacuo
- additionCH2Cl2/ether (1:2, 5 mL) was added
- customfollowed by sonication
- customthe precipitation
- filtrationwas filtered as 138c