HRID729596

反应详情

EQUATION

反应方程式

HRID 729596 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Heat a mixture of 4,4,5,5,5-pentafluoro-3-oxo-pentanenitrile (4 g, 21.4 mmol) and p-tolyl-hydrazine (10 g, 64.1 mmol) in ethanol (20 mL) to 95° C. in a sealed tube apparatus for 15 hours. After cooling to room temperature, remove the solvent under reduced pressure to give a brown residue. Subject residue to silica gel chromatography eluting with ethyl acetate and hexanes to give the title compound (3.24 g, 52% yield, ES+(m/z) 292.1 [M+H]).

WORKUP

后处理

  1. temperatureHeat
  2. customremove the solvent under reduced pressure
  3. customto give a brown residue
  4. washSubject residue to silica gel chromatography eluting with ethyl acetate and hexanes