HRID1157153

反应详情

EQUATION

反应方程式

HRID 1157153 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 2-fluoro-5-nitrobenzotrifluoride (500 mg, 2.48 mmol) and benzyl alcohol (267 mg, 2.48 mmol) in THF was added sodium hydride (95.1 mg, 2.48 mmol) at 0° C. The reaction was followed by TLC and quenched with saturated ammonium chloride solution after 0.5 h. The mixture was extracted with dichloromethane three times. The combined organic layer was dried over sodium sulfate and concentrated. The residue was triturated with 2.5 mL of hexanes and ethyl acetate (7:1) and a yellow precipitate was collected by filtration to give 1-benzyloxy-4-nitro-2-trifluoromethylbenzene (580 mg, 79%).

WORKUP

后处理

  1. customquenched with saturated ammonium chloride solution after 0.5 h
  2. extractionThe mixture was extracted with dichloromethane three times
  3. dry with materialThe combined organic layer was dried over sodium sulfate
  4. concentrationconcentrated
  5. customThe residue was triturated with 2.5 mL of hexanes and ethyl acetate (7:1)
  6. filtrationa yellow precipitate was collected by filtration