HRID392453

反应详情

EQUATION

反应方程式

HRID 392453 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

PROCEDURE

实验过程

A solution of N-(3-bromophenyl)pyridin-3-ylmethylamine (364 mg, 1.38 mmol), 4-cyanophenylboronic acid (305 mg, 2.08 mmol), sodium carbonate (2.15 ml of a 2M aqueous solution, 4.3 mmol), and tetrakis(triphenylphosphine)palladium(0) (70 mg, 0.061 mmol), under a nitrogen atmosphere was refluxed in dioxane (15 ml) for 6 h, then cooled to room temperature. The mixture was diluted with dichloromethane (70 ml) and water (15 ml). The organics were separated, dried over sodium sulfate, filtered, and concentrated to a brown solid. The solid was purified by radial chromatography eluting with 2 to 4% methanol/dichloromethane to afforded the title compound. MS calcd. 285.3; MS (M+1) 286.3.

WORKUP

后处理

  1. customThe organics were separated
  2. dry with materialdried over sodium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated to a brown solid
  5. customThe solid was purified by radial chromatography
  6. washeluting with 2 to 4% methanol/dichloromethane