HRID1860589

反应详情

EQUATION

反应方程式

HRID 1860589 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-Hydrazino-5-(methylsulfonyl)pyridine hydrochloride (128 mg, 0.54 mmol) and 4,4,4-trifluoro-1-(1-cyclohexenyl)-1,3-butanedione (100 mg, 0.45 mmol) were mixed in ethanol (8 ml). The resulting reaction mixture was heated at reflux temperature for 35 hours. The solvent was then removed in vacuo, and the residue was partitioned between EtOAc and water. The organic layer was washed with brine and concentrated in vacuo. The product was purified by flash chromatography using methylene chloride to give the title compound (30.6 mg, 18%).

WORKUP

后处理

  1. customThe resulting reaction mixture
  2. temperaturewas heated
  3. temperatureat reflux temperature for 35 hours
  4. customThe solvent was then removed in vacuo
  5. customthe residue was partitioned between EtOAc and water
  6. washThe organic layer was washed with brine
  7. concentrationconcentrated in vacuo
  8. customThe product was purified by flash chromatography