HRID1027173

反应详情

EQUATION

反应方程式

HRID 1027173 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

A mixture of 2-(2-pyridyl)benzimidazole (287 mg, 1.469 mmol), cesium carbonate (5.98 g, 18.36 mmol), copper(I) iodide (280 mg, 1.469 mmol) and DMF (5 mL) were combined in a microwave vial fitted with an N2 inlet and magnetic stir bar. The slurry was heated at 60° C. for 1 h, followed by addition of imidazole (500 mg, 7.34 mmol) and 1-bromo-4-iodo-2-methoxybenzene (2.3 g, 7.34 mmol). The reaction mixture was heated at 90° C. for 2 days. The reaction mixture was filtered through celite, washed with EtOAc, and concentrated in vacuo. The crude material was purified by silica gel chromotography (10% to 40% EtOAc in heptanes) to give 1-(4-bromo-3-methoxyphenyl)-1H-imidazole (1.25 g, MS: 255.2 [M+H+])

WORKUP

后处理

  1. customvial fitted with an N2 inlet and magnetic stir bar
  2. temperatureThe reaction mixture was heated at 90° C. for 2 days
  3. filtrationThe reaction mixture was filtered through celite
  4. washwashed with EtOAc
  5. concentrationconcentrated in vacuo
  6. customThe crude material was purified by silica gel chromotography (10% to 40% EtOAc in heptanes)