HRID579912

反应详情

EQUATION

反应方程式

HRID 579912 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
65 °C

PROCEDURE

实验过程

To a reactor is added 30 ml of H2O and 15 g of 50% aqueous NaOH. The solution is heated to 65° C. and 3.85 g (0.051 mol) of cobalt oxide and 5 g (0.022 mol) of 2-methyl-3-quinolinecarboxylic acid hydrochloride are added with stirring. A chilled solution of 13 g (0.18 mol) of chlorine in 40 g of chlorine in 40 g of 25% aqueous NaOH (~24% aqueous NaOCl) is added over 3 hours. The solution is then stirred for 15 hours and an additional aliquot of 24% aqueous NaOCl (0.36 mol total) is added over 3 hours. After a total of 36 hours, the solution is filtered, chilled to 15° C. and acidified to pH 3. The solid material is removed by filtration. A product of 2.3 g of 2,3-quinolinedicarboxylic acid is obtained. This represents a yield of 77% based on consumed 2-methyl-3-quinolinecarboxylic acid. The reaction is illustrated as follows: ##STR13##

WORKUP

后处理

  1. stirringThe solution is then stirred for 15 hours
  2. filtrationAfter a total of 36 hours, the solution is filtered
  3. temperaturechilled to 15° C.
  4. customThe solid material is removed by filtration