HRID917620

反应详情

EQUATION

反应方程式

HRID 917620 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
140 °C

PROCEDURE

实验过程

2-Cyano-3,5-dibromopyridine (prepared in the above (2)) 3.27 g is added to a mixture of acetic acid 14 ml, sulfuric acid 14 ml and water 14 ml, and the mixture is refluxed at 140° C. for 4 hours. The reaction mixture is cooled and water is added thereto. The resulting precipitate is filtered and washed with water. The precipitate is dissolved in ether, washed and dried. The solvent is removed in vacuo and crystallized from a mixture of ether and hexane to give 3,5-dibromopyridine-2-carboxylic acid. mp 170-171° C.

WORKUP

后处理

  1. temperatureThe reaction mixture is cooled
  2. filtrationThe resulting precipitate is filtered
  3. washwashed with water
  4. dissolutionThe precipitate is dissolved in ether
  5. washwashed
  6. customdried
  7. customThe solvent is removed in vacuo
  8. customcrystallized from a mixture of ether and hexane