HRID2218419

反应详情

EQUATION

反应方程式

HRID 2218419 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
105 °C

PROCEDURE

实验过程

2,3-Diamino-4,5-dichloropyridine (Example 206a) (2.5 g, 14 mmol) and 4-nitrobenzoic acid (2.3 g, 14 mmol) were dissolved in POCl3 (40 ml) and heated to 105° C. for 5 h. The excess of POCl3 was evaporated off and the residue was dissolved in EtOAc and aqueous K2CO3. The aqueous phase was basified with 10M KOH and extracted three times with EtOAc. The combined organic phase was washed with brine, dried (Na2SO4) and evaporated in vacuo to afford the title compound (2.5 g, 58%).

WORKUP

后处理

  1. customThe excess of POCl3 was evaporated off
  2. dissolutionthe residue was dissolved in EtOAc
  3. extractionextracted three times with EtOAc
  4. washThe combined organic phase was washed with brine
  5. dry with materialdried (Na2SO4)
  6. customevaporated in vacuo