HRID424863

反应详情

EQUATION

反应方程式

HRID 424863 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of N-(5-chloro-2-nitrophenyl)-N-methylamine (8.00 g) in N,N-dimethylacetamide (112 ml) was added 2,6-di-t-butyl-4-methylphenol (0.24 g). Furthermore, to the resulting mixture were added 4-amino-3,5-dimethylphenol (6.47 g) and potassium t-butoxide (5.29 g) with stirring, and the resulting mixture was stirred at 60° C. for 30 minutes. After stirring, water (4 ml) was added to the reaction mixture, and furthermore water (120 ml) was added dropwise over a 2-hour interval, and then the resulting mixture was cooled gradually to room temperature. The crystalline solid precipitated was collected by filtration, washed with water (80 ml) and dried in vacuo to afford the title compound (11.45 g, yield: 93%) as a yellow crystalline solid.

WORKUP

后处理

  1. stirringthe resulting mixture was stirred at 60° C. for 30 minutes
  2. stirringAfter stirring
  3. additionwas added dropwise over a 2-hour interval
  4. customThe crystalline solid precipitated
  5. filtrationwas collected by filtration
  6. washwashed with water (80 ml)
  7. customdried in vacuo