HRID270800

反应详情

EQUATION

反应方程式

HRID 270800 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a suspension of zinc dust (1.5 g) in glacial acetic acid (10 mL) was added drop-wise, a solution of 3-Heptafluoropropyl-5-methyl-4-nitro-1H-pyrazole (0.295 g, 1.0 mmol) in glacial acetic acid (5 mL). The reaction mixture was then allowed to stir at room temperature for 14 h. The zinc salts were then removed by filtration and the residue washed with ethyl acetate. The combined organic extract was concentrated in vacuum, re-dissolved in CHCl3, washed with NaHCO3, water and brine. Finally the organic layer was dried with Na2SO4 and solvent evaporated to give the title compound as white solid.

WORKUP

后处理

  1. additionwas added drop-wise
  2. customThe zinc salts were then removed by filtration
  3. washthe residue washed with ethyl acetate
  4. extractionThe combined organic extract
  5. concentrationwas concentrated in vacuum
  6. dissolutionre-dissolved in CHCl3
  7. washwashed with NaHCO3, water and brine
  8. dry with materialFinally the organic layer was dried with Na2SO4 and solvent
  9. customevaporated