HRID2202913

反应详情

EQUATION

反应方程式

HRID 2202913 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

A mixture of 4-((4-chlorobenzyl)oxy)pyridin-2(1H)-one (10 g), 5-bromo-N-methyl-2-nitroaniline (9.80 g), N,N′-dimethylethylenediamine (4.76 ml), copper iodide (8.08 g), potassium carbonate (17.59 g) and DMSO (200 ml) was heated at 150° C. for 2 h. The mixture was poured into 28% NH3 solution. The resulting precipitate was collected and washed with IPA. The solid was dissolved in DMSO (100 ml) at 80° C., and allowed to cool to room temperature to give a precipitate. After filtration, the precipitate was washed with IPA and dried to give the title compound (12 g) as a yellow solid.

WORKUP

后处理

  1. customThe resulting precipitate was collected
  2. washwashed with IPA
  3. dissolutionThe solid was dissolved in DMSO (100 ml) at 80° C.
  4. temperatureto cool to room temperature
  5. customto give a precipitate
  6. filtrationAfter filtration
  7. washthe precipitate was washed with IPA
  8. customdried