HRID2203037

反应详情

EQUATION

反应方程式

HRID 2203037 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-(benzyloxy)pyridin-2(1H)-one (1.0 g), 6-bromo-2-ethyl-1-methyl-1H-benzimidazole (1.19 g), potassium carbonate (2.06 g), N,N′-dimethylethylenediamine (0.53 ml), CuI (0.95 g) and DMSO (20 ml) was stirred at 150° C. for 2 h. After cooling to 0° C., 28% NH3 solution (56.0 ml) was added. The precipitate was collected by filtration. The collected material was dissolved in THF, passed through a plug of NH silica gel (EtOAc) and concentrated in vacuo. The resulting solid was collected to give the title compound (1.03 g) as a pink solid.

WORKUP

后处理

  1. temperatureAfter cooling to 0° C.
  2. filtrationThe precipitate was collected by filtration
  3. dissolutionThe collected material was dissolved in THF
  4. concentrationconcentrated in vacuo
  5. customThe resulting solid was collected