HRID1875052

反应详情

EQUATION

反应方程式

HRID 1875052 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Sodium hydride (60% oil dispersion) (2.125 g, 53.1 mmol) was added in portions to a solution of phenol (5.00 g, 53.1 mmol) in THF (100 mL) while cooling in an ice bath. After 30 min, 1,2,3-trifluoro-4-nitrobenzene (6.11 mL, 53.1 mmol) was added. The mixture was stirred at RT overnight. The reaction mixture was poured on to ice/10% aqueous HCl and extracted with ethyl acetate. The organic layer was dried over sodium sulfate and the solvent was evaporated. Chromatography of the residue (ethyl acetate:hexane) gave the crude product (10.78 g, 43%) as a yellow oil.

WORKUP

后处理

  1. temperaturewhile cooling in an ice bath
  2. extractionextracted with ethyl acetate
  3. dry with materialThe organic layer was dried over sodium sulfate
  4. customthe solvent was evaporated