HRID77067

反应详情

EQUATION

反应方程式

HRID 77067 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
170 °C

PROCEDURE

实验过程

Method 2—Step a Into a one necked round bottomed flask equipped with a magnetic stirrer, 5-bromo-2-chlorobenzoic acid (70.0 g, 297.3 mmol), o-phenylenediamine (64.3 g, 594.6 mmol) and methansulfonic acid (140 mL) were placed and heated to 170° C. in order to melt the solids. The system was stirred 5 h at this temperature, then left to come rt. The blue solid was treated with NaOH 35% (200 mL) obtaining a violet suspension (pH 5) that was filtered and washed with NaOH 0.5 M (2 L) and H2O (2 L). The product was dried under vacuum (60° C.), to give 61.6 g of a pure violet solid. (67%).

WORKUP

后处理

  1. customMethod 2—Step a Into a one necked round bottomed flask equipped with a magnetic stirrer
  2. waitleft
  3. customto come rt