HRID2266741

反应详情

EQUATION

反应方程式

HRID 2266741 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A mixture of 5-iodo-4′-methyl-biphenyl-3-carboxylic acid methyl ester (2.0 g, 5.7 mmol), 2-ethyl-imidazole (1.1 g, 11.4 mmol), (L)-proline (0.26 g, 2.28 mmol), CuI (0.22 g, 1.14 mmol) and K2CO3 (1.57 g, 11.4 mmol) in DMSO (30 mL) was flushed with N2, then heated to 100° C. overnight. After cooling to room temperature, the reaction mixture was extracted with EtOAc. The combined organic layers were separated, washed with water, dried over anhydrous sodium sulfate, filtered, and concentrated under reduced pressure. The residue was purified by flash chromatography to afford 5-(2-ethyl-imidazol-1-yl)-4′-methyl-biphenyl-3-carboxylic acid methyl ester as a white solid (750 mg, 41.1%).

WORKUP

后处理

  1. customwas flushed with N2
  2. temperatureAfter cooling to room temperature
  3. extractionthe reaction mixture was extracted with EtOAc
  4. customThe combined organic layers were separated
  5. washwashed with water
  6. dry with materialdried over anhydrous sodium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressure
  9. customThe residue was purified by flash chromatography