HRID2044201

反应详情

EQUATION

反应方程式

HRID 2044201 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of N,N-dimethyl-5-ethyl-2-iodophenylacetamide (2.0 g, 6.3 mmol), 2-fluoro-methyl-3-trifluoromethylaniline (2.4 g, 12.6 mmol), copper (0.2 g, 3.2 mmol), cuprous iodide (0.6 g, 3.2 mmol), and K2CO3 (0.9 g, 6.3 mmol) in xylenes (6.0 mL) are heated at reflux for 24 h. After cooling, the crude reaction mixture is diluted with EtOAc and filtered through Celite®. The filtrate is concentrated under reduced pressure. The residue is purified by flash chromatography, eluting with hexanes, then up to 25% EtOAc/hexane mixtures to give the target compound 5-ethyl-2-(2′-fluoro-4′-methyl-3′-trifluoromethylanilino)phenylacetic acid N,N-dimethyl amide.

WORKUP

后处理

  1. temperatureare heated
  2. temperatureat reflux for 24 h
  3. temperatureAfter cooling
  4. customthe crude reaction mixture
  5. filtrationfiltered through Celite®
  6. concentrationThe filtrate is concentrated under reduced pressure
  7. customThe residue is purified by flash chromatography
  8. washeluting with hexanes