HRID563923

反应详情

EQUATION

反应方程式

HRID 563923 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of 762 mg (2.23 mmol) N-[2-(5-methyl-thiophen-2-yl)-ethyl]-3-(4-trifluoromethyl-phenyl)-propionamide in 10 mL acetonitrile was added 460 uL (4.91 mmol) POCl3. The mixture was heated to reflux for 1 h and the solvent was removed in vacuo. The residue was taken up in toluene and concentrated again in vacuo. The oil was dissolved in dichloromethane and was basified with sat. NaHCO3. The organic layer was dried over Na2SO4, filtered and concentrated in vacuo. 740 mg of the title compound was isolated which was used without further purification in the consecutive step.

WORKUP

后处理

  1. temperatureThe mixture was heated
  2. temperatureto reflux for 1 h
  3. customthe solvent was removed in vacuo
  4. concentrationconcentrated again in vacuo
  5. dissolutionThe oil was dissolved in dichloromethane
  6. dry with materialThe organic layer was dried over Na2SO4
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo