HRID642090

反应详情

EQUATION

反应方程式

HRID 642090 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of methyl 4-(aminomethyl)benzoate (75 g, 0.46 mol) and TEA (315 mL, 2.27 mol) in anhydrous DCM (1.5 L) was added a solution of freshly prepared 4-chloro benzoyl chloride (0.91 mol) in DCM (400 mL). The resulting mixture was allowed to stir for 12 hrs. The reaction was quenched with a 10% aqueous solution of sodium hydrogenocarbonate. The organic layer was washed with a 1.5N HCl solution and water. After drying over MgSO4 and evaporation of the solvent in vacuo, a solid was obtained. Recrystallization form MeOH gave the title compound (80 g) in a 60% yield as a white powder.

WORKUP

后处理

  1. customThe reaction was quenched with a 10% aqueous solution of sodium hydrogenocarbonate
  2. washThe organic layer was washed with a 1.5N HCl solution and water
  3. dry with materialAfter drying over MgSO4 and evaporation of the solvent in vacuo
  4. customa solid was obtained
  5. customRecrystallization
  6. customform MeOH