HRID431878

反应详情

EQUATION

反应方程式

HRID 431878 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In a 100 ml round bottom flask equipped with stir bar added Methyl-3-bromo-5-(3-pyridyl)benzoate (1.16 g, 3.96 mmol), methanol (15 ml) and sodium hydroxide (5.94 ml, 5.94 mmol, 1N aqueous). Stirred the resulting mixture at 50° C. for 2 h. The reaction mixture was cooled to room temperature, concentrated in-vacuo and the residue was dissolved in methanol (20 ml). To this mixture added hydrochloric acid (1N diethyl ether) dropwise and stirred at room temperature for 10 min. The reaction mixture was concentrated in-vacuo and the residue was triturated with diethyl ether to provide the crude hydrochloride salt of title compound (1.50 g) as a white solid.

WORKUP

后处理

  1. customIn a 100 ml round bottom flask equipped
  2. stirringStirred the resulting mixture at 50° C. for 2 h
  3. concentrationconcentrated in-vacuo
  4. dissolutionthe residue was dissolved in methanol (20 ml)
  5. additionTo this mixture added hydrochloric acid (1N diethyl ether) dropwise
  6. stirringstirred at room temperature for 10 min
  7. concentrationThe reaction mixture was concentrated in-vacuo
  8. customthe residue was triturated with diethyl ether