HRID6898

反应详情

EQUATION

反应方程式

HRID 6898 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
105 °C

PROCEDURE

实验过程

A flame-dried flask containing N2 inlet and magnetic stirrer was charged with 2.9 g (18 mmol) of 3,4-dichlorophenol, 6.2 g (45 mmol) of potassium carbonate and 50 mL of anhydrous DMF. With stirring, 2.08 g (15 mmol) of 2,5-difluorobenzonitrile (Aldrich Chem. Co.) was added and the mixture was heated overnight at 105° C., cooled to room temperature and partitioned between water and EtOAc. The aqueous layer was reextracted with EtOAc and the combined organic layers were successively washed with 2N NaOH, water and saturated aqueous NaCl. After drying with MgSO4, the solvent was removed to give the title product as a light brown oil which slowly solidified, 3.5 g.

WORKUP

后处理

  1. additionA flame-dried flask containing N2 inlet and magnetic stirrer
  2. temperaturecooled to room temperature
  3. custompartitioned between water and EtOAc
  4. washthe combined organic layers were successively washed with 2N NaOH, water and saturated aqueous NaCl
  5. dry with materialAfter drying with MgSO4
  6. customthe solvent was removed