HRID488791

反应详情

EQUATION

反应方程式

HRID 488791 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
23 °C

PROCEDURE

实验过程

A solution of 5-methyl-2-phenyl-2H-1,2,3-triazole-4-carboxylic acid (10.2 g, 50 mmol) and NaOH (17.6 g, 440 mmol) in water (375 mL) at 23° C. was treated with KMnO4 (30.8 g, 195 mmol). The resulting solution was heated at reflux for 17 h, cooled to 23° C. and treated with ethanol (50 mL). The resulting mixture was filtered to remove MnO2. The filtrate was acidified with HCl (conc.) to pH 1. The resulting white solid was collected by filtration. The filtrate was concentrated to half volume and more solid was collected by filtration. The two combined batches of solid were dried in vacuo to afford 11.1 g (95%) of 2-phenyl-2H-1,2,3-triazole-4,5-dicarboxylic acid.

WORKUP

后处理

  1. temperatureThe resulting solution was heated
  2. temperatureat reflux for 17 h
  3. filtrationThe resulting mixture was filtered
  4. customto remove MnO2
  5. filtrationThe resulting white solid was collected by filtration
  6. concentrationThe filtrate was concentrated to half volume and more solid
  7. filtrationwas collected by filtration
  8. customThe two combined batches of solid were dried in vacuo