HRID2357855

反应详情

EQUATION

反应方程式

HRID 2357855 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

The mixture of 1,4-diiodobenzene 1-1 (600 mg, 1.8 mmol), 2-methyl-1H-imidazole-4-carbaldehyde (200 mg, 1.8 mmol), K2CO3 (503 mg, 3.6 mmol), CuI (105 mg, 0.55 mmol) and 8-hydroxyquinoline (80 mg, 0.55 mol) in 5 mL DMSO and 5 mL dioxane in a sealed tube was stirred for 2 days at 120° C. It was cooled to rt, and to it was added 60 mL water. The mixture was stirred for 30 min and filtered through a celite layer. The filtrate was concentrated in vacuo and subjected to reverse phase preparative HPLC to isolate 1-(4-iodophenyl)-2-methyl-1H-imidazole-4-carbaldehyde 5-1. MS found for C11H9IN2O (M+H)+313.0.

WORKUP

后处理

  1. temperatureIt was cooled to rt
  2. stirringThe mixture was stirred for 30 min
  3. filtrationfiltered through a celite layer
  4. concentrationThe filtrate was concentrated in vacuo