HRID2209462

反应详情

EQUATION

反应方程式

HRID 2209462 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of N-bromosuccinimide (1.4 gm) in 10 mL dimethylformamide was added in a dropwise manner to a solution of 4-(4-aminobenzyl)pyridine (1.5 gm) in 10 mL of dimethylformamide. The reaction flask was wrapped in aluminum foil to prevent exposure of the reagents to light. The reaction mixture was stirred at room temperature for 3 hours. The progress of the reaction was monitored by thin-layer chromatography. When the reaction was completed, the reaction mixture was combined with 100 mL of H2O with stirring. A reddish brown precipitate was formed, filtered out of solution, washed with H2O, and air dried. The solid was dissolved in ethyl acetate, back washed with saturated NaCl, dried over MgSO4 and triturated with ethyl ether. The solid was filtered from the solution and air dried yielding 1.6 gm of 4-(4-amino-3-bromobenzyl)pyridine as reddish/tan crystals.

WORKUP

后处理

  1. stirringwith stirring
  2. customA reddish brown precipitate was formed
  3. filtrationfiltered out of solution
  4. washwashed with H2O, and air
  5. customdried
  6. dissolutionThe solid was dissolved in ethyl acetate
  7. washback washed with saturated NaCl
  8. dry with materialdried over MgSO4
  9. customtriturated with ethyl ether
  10. filtrationThe solid was filtered from the solution and air
  11. customdried