HRID1874780

反应详情

EQUATION

反应方程式

HRID 1874780 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The crude {3-[(3-chloro-5-cyanophenyl)oxy]-2-fluoro-4-nitrophenyl}acetic acid was dissolved in CH3CN (50 mL) and Cu2O (0.65 g, 4.5 mmol) was added. A condenser was attached and the heterogeneous mixture was heated to reflux for 2 h. The reaction mixture was cooled to RT, filtered through Celite and the solvent evaporated. Purification was accomplished by column chromatography (hexane/EtOAc) to afford the title compound (6.0 g, 87%), which solidified upon standing. 1H NMR (400 MHz, DMSO-d6): δ ppm 7.98 (dd, 1H), 7.81 (d, 1H), 7.60 (d, 2H), 7.52 (t, 1H), 2.37 (d, 3H).

WORKUP

后处理

  1. customA condenser was attached
  2. temperaturethe heterogeneous mixture was heated
  3. temperatureto reflux for 2 h
  4. filtrationfiltered through Celite
  5. customthe solvent evaporated
  6. customPurification