HRID2051380

反应详情

EQUATION

反应方程式

HRID 2051380 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
30 °C

PROCEDURE

实验过程

A mixture of 4-bromo-1-acetylaminoanthraquinone (purity 98%, 35.1 g), methyl isobutyl ketone (500 g), tetra-n-butyl ammonium bromide (0.3 g) and 96% potassium hydroxide (12.0 g) was stirred for 1 hour while being maintained at 30° C. Dimethylsulfuric acid (25.2 g) was dropped at 30° C. over 2 hours. The mixture was stirred at 30° C. for 1 hour, 40° C. for 2 hours and 50° C. for 4 hours, successively. After water (250 g) was added, the solution was stirred for 1 hour, while being maintained at 50° C. Then, the same procedure as in Example 3 was applied to obtain, after methyl isobutyl ketone was recovered, 4-bromo-N-acetyl-1-methylaminoanthraquinone (34.8 g, purity 93.6%, yield 91.0%).

WORKUP

后处理

  1. stirringThe mixture was stirred at 30° C. for 1 hour, 40° C. for 2 hours and 50° C. for 4 hours
  2. stirringthe solution was stirred for 1 hour
  3. temperaturewhile being maintained at 50° C
  4. customto obtain
  5. customafter methyl isobutyl ketone was recovered