HRID1160837

反应详情

EQUATION

反应方程式

HRID 1160837 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
125 °C

PROCEDURE

实验过程

To a solution of N-(5-chloro-2-nitrophenyl)-N-methylamine (0.86 g) and 3,5-dimethyl-4-nitrophenol (0.76 g) in N,N-dimethylacetamide (12 ml) was added potassium t-butoxide (0.554 g) at room temperature, and the resulting mixture was stirred successively at the same temperature for 20 minutes, at 100° C. for 10 minutes, at 125° C. for 45 minutes, and at 140° C. for 1 hour. After cooling the reaction mixture to 0° C., the reaction mixture was adjusted to a pH of about 3 with 3N hydrochloric acid. The crystalline solid precipitated was collected by filtration, washed successively with 3N hydrochloric acid and water and air-dried for 3 days to afford the title compound (1.16 g, yield: 80%).

WORKUP

后处理

  1. waitat 140° C. for 1 hour
  2. temperatureAfter cooling the reaction mixture to 0° C.
  3. customThe crystalline solid precipitated
  4. filtrationwas collected by filtration
  5. washwashed successively with 3N hydrochloric acid and water
  6. customair-dried for 3 days