HRID402759

反应详情

EQUATION

反应方程式

HRID 402759 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of ethyl 3-oxo-3-(2,4,5-trifluorophenyl)propanoate (0.326 g, 1.32 mmol) and N,N-dimethyformamide dimethyl acetal in ethanol (5 mL) was heated in a 90° C. oil bath for 3 hours. Upon removal of the volatiles, the residue was dissolved in EtOH (3 mL) and phenylhydrazine hydrochloride salt (191 mg, 1.324 mmol) was added. The mixture was then heated at reflux for 6 hours. The reaction was cooled and diluted with EtOAc and the organic layer was washed with NaHCO3 and brine. The organic phase was dried with Na2SO4, filtered and concentrated to afford the title compound as oil.

WORKUP

后处理

  1. customUpon removal of the volatiles
  2. dissolutionthe residue was dissolved in EtOH (3 mL)
  3. temperatureThe mixture was then heated
  4. temperatureat reflux for 6 hours
  5. temperatureThe reaction was cooled
  6. washthe organic layer was washed with NaHCO3 and brine
  7. dry with materialThe organic phase was dried with Na2SO4
  8. filtrationfiltered
  9. concentrationconcentrated