HRID1845221

反应详情

EQUATION

反应方程式

HRID 1845221 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. customirradiation at 120° C. for 2 hours
  2. temperatureThe mixture was cooled
  3. customto precipitate
  4. washthe precipitated solids were rinsed with hexane
  5. custompurified by preparative HPLC (100×21.2 mm C18 column, 30-70% CH3CN/water[10 mM Et2NH])
  6. customto afford a white foam