HRID1860589
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customThe resulting reaction mixture
- temperaturewas heated
- temperatureat reflux temperature for 35 hours
- customThe solvent was then removed in vacuo
- customthe residue was partitioned between EtOAc and water
- washThe organic layer was washed with brine
- concentrationconcentrated in vacuo
- customThe product was purified by flash chromatography