HRID1972254

反应详情

EQUATION

反应方程式

HRID 1972254 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

To a dry round bottom flask is added [2-hydroxy-1-(3-methoxy-phenyl)ethyl]-carbamic acid benzyl ester (300 mg, 1 mmol), 1-(4-chlorophenoxy)-4-iodobenzene (330 mg, 1 mmol), K3PO4 (210 mg), 1,2-cyclohexanediamine (15 μL) and CuI (20 mg), and DMF (5 mL). The mixture is evacuated and back-filled with nitrogen three times. The reaction mixture is heated to 110° C. for 7 h. The reaction is then cooled to room temperature, diluted with EtOAc (50 mL), washed with 1N HCl, and brine, subsequently dried over MgSO4, filtered, and concentrated to give the crude product, which is purified by flash chromatography on silica gel (EtOAc/Hex: 1/2) to provide 3-[4-(4-chlorophenoxy)phenyl]-4-(3-methoxyphenyl)-oxazolidin-2-one (304 mg).

WORKUP

后处理

  1. customThe mixture is evacuated
  2. additionback-filled with nitrogen three times
  3. temperatureThe reaction is then cooled to room temperature
  4. additiondiluted with EtOAc (50 mL)
  5. washwashed with 1N HCl, and brine
  6. dry with materialsubsequently dried over MgSO4
  7. filtrationfiltered
  8. concentrationconcentrated
  9. customto give the crude product, which
  10. customis purified by flash chromatography on silica gel (EtOAc/Hex: 1/2)