HRID1166720

反应详情

EQUATION

反应方程式

HRID 1166720 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Methyl-3-cyano-4-hydroxybenzoate (2.71 g, 15.3 mmol) was dissolved in 50 mL of THF. The solution was chilled in an ice bath, and 2.0M potassium hydroxide (17 mL, 34 mmol) was added dropwise. The resulting mixture was stirred at room temperature overnight. TLC indicated complete reaction. The THF was removed by rotary evaporation. The aqueous residue was acidified with aqueous trifluoroacetic acid and purified by reverse-phase HPLC (C-18, 0.1% TFA in water and acetonitrile). 3-Cyano-4-hydroxybenzoic acid was obtained as a white powder (2.1 g, 84%) after lyophilization.

WORKUP

后处理

  1. temperatureThe solution was chilled in an ice bath
  2. customreaction
  3. customThe THF was removed by rotary evaporation
  4. custompurified by reverse-phase HPLC (C-18, 0.1% TFA in water and acetonitrile)