反応 #519060

反応方程式

Methyl-3-bromo-5-(3-pyridyl)benzoate

sodium hydroxide

→

title compound

収率 136.2%

3-Bromo-5-(3-pyridyl)benzoic Acid

収率 136.2%

溶媒

methanol

反応条件

後処理

1. 1
   その他In a 100 ml round bottom flask equipped
2. 2
   workup.STIRRINGStirred the resulting mixture at 50° C. for 2 h
3. 3
   濃縮concentrated in-vacuo
4. 4
   workup.DISSOLUTIONthe residue was dissolved in methanol (20 ml)
5. 5
   workup.ADDITIONTo this mixture added hydrochloric acid (1N diethyl ether) dropwise
6. 6
   workup.STIRRINGstirred at room temperature for 10 min
7. 7
   濃縮The reaction mixture was concentrated in-vacuo
8. 8
   その他the residue was triturated with diethyl ether

実験手順

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.

出典