HRID1844777

反应详情

EQUATION

反应方程式

HRID 1844777 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
2.5 °C

PROCEDURE

实验过程

45 g (0.25 mol) 4-Amino-3-nitrobenzoic acid, 400 ml water and 100 ml concentrated hydrochloric acid were added into a reaction flask. Started to stir, and the mixture was cooled to 0 to 5° C., then 50 ml aqueous solution of 25.9 g sodium nitrite (0.38 mol) was added dropwise. The solid was dissolved gradually. After completing the dropwise addition, the mixture was reacted at 0 to 5° C. for 1 hour, and 200 ml aqueous solution of 88 g (0.5 mol) potassium iodide was added dropwise at this temperature. The mixture was stirred at room temperature for 2 h after completing the dropwise addition, and solid was precipitated. The solid was filtered, washed with water, and dried to obtain 4-iodo-3-nitrobenzoic acid (compound V) as a solid, 65 g (0.22 mol), yield 89.7%.

WORKUP

后处理

  1. dissolutionThe solid was dissolved gradually
  2. additionthe dropwise addition
  3. customthe mixture was reacted at 0 to 5° C. for 1 hour
  4. stirringThe mixture was stirred at room temperature for 2 h
  5. additionthe dropwise addition, and solid
  6. customwas precipitated
  7. filtrationThe solid was filtered
  8. washwashed with water
  9. customdried