HRID565131

反应详情

EQUATION

反应方程式

HRID 565131 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In 30 ml of DMF, 2.9 g of the compound (3) obtained in Example 3 were dissolved, followed by the addition of 0.59 g of 4-aminomethylpyridine. The resultant mixture was stirred at room temperature, to which 0.60 g of t-BuOK was added under ice cooling. The thus-obtained mixture was stirred at room temperature for 5 hours. The DMF was distilled off under reduced pressure, and the residue was dissolved in CHCl3. The solution so obtained was washed with water and then dried over anhydrous magnesium sulfate (MgSO4). The solvent was distilled off under reduced pressure. The residue was isolated and purified by chromatography on a silica gel column (eluent: CHCl3/MeOH=7/3), whereby 0.41 g of the compound (4) was obtained (yield: 18%).

WORKUP

后处理

  1. additionwas added under ice cooling
  2. distillationThe DMF was distilled off under reduced pressure
  3. dissolutionthe residue was dissolved in CHCl3
  4. customThe solution so obtained
  5. washwas washed with water
  6. dry with materialdried over anhydrous magnesium sulfate (MgSO4)
  7. distillationThe solvent was distilled off under reduced pressure
  8. customThe residue was isolated
  9. custompurified by chromatography on a silica gel column (eluent: CHCl3/MeOH=7/3)