HRID130324

反应详情

EQUATION

反应方程式

HRID 130324 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

To a heated mixture (in an oversized flask) of 13 g (63 mmol) 4,6-dimethoxyindole-2,3-dione prepared in Example 1 and 108 ml of 33% NaOH solution was carefully added 20 ml of a 30% solution of H2O2. A vigorous exothermic reaction occurs. After all H2O2 was added, the reaction mixture was maintained at 100° C. for an additional 10 min. The pH of the solution was brought to 8 with concentrated HCl and acidified to pH 5-6 with acetic acid. The solid was filtered, washed with water and dried to yield 6.2 g of 4,6-dimethoxyanthranilic acid as a pale brown solid (50% yield).

WORKUP

后处理

  1. customA vigorous exothermic reaction
  2. filtrationThe solid was filtered
  3. washwashed with water
  4. customdried