HRID1845221
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 mixture of 3-bromo-N-((6-methylpyridin-3-yl)methyl)-5-(methylsulfonyl)benzamide (71 mg, 0.18 mmol), 5-methyl-2-(tributylstannyl)pyridine (91 mg, 0.23 mmol), tetrakis(triphenylphosphine)palladium(0) (11 mg, 0.0093 mmol) and toluene (2.0 mL) under argon was subjected to microwave irradiation at 120° C. for 2 hours. The mixture was cooled to allow the product to precipitate. The solvent was discarded and the precipitated solids were rinsed with hexane and then purified by preparative HPLC (100×21.2 mm C18 column, 30-70% CH3CN/water[10 mM Et2NH]) to afford a white foam.
WORKUP
后处理
- customirradiation at 120° C. for 2 hours
- temperatureThe mixture was cooled
- customto precipitate
- washthe precipitated solids were rinsed with hexane
- custompurified by preparative HPLC (100×21.2 mm C18 column, 30-70% CH3CN/water[10 mM Et2NH])
- customto afford a white foam