HRID1269860

反应详情

EQUATION

反应方程式

HRID 1269860 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Anhydrous trifluoromethanesulfonate (3.17 ml, 18.8 mmol) and triethylamine (2.75 ml, 19.7 mmol) were added dropwise to a solution of 2,3-dimethyl-4-nitrophenol (3.0 g, 17.9 mmol) in methylene chloride (60 ml) at 0° C. and stirred at room temperature for 1 hour. Then, the reaction solution was poured into water and extracted with chloroform. The organic layer was dried over magnesium sulfate and distilled to remove the solvent, and the resulting residue was purified by a silica gel column chromatography (eluent: hexane/ethyl acetate) to obtain 2,3-dimethyl-4-nitrophenyl trifluoromethanesulfonate (5.32 g, 99%).

WORKUP

后处理

  1. extractionextracted with chloroform
  2. dry with materialThe organic layer was dried over magnesium sulfate
  3. distillationdistilled
  4. customto remove the solvent
  5. customthe resulting residue was purified by a silica gel column chromatography (eluent: hexane/ethyl acetate)