HRID730425
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
To a solution of 5-amino-1-[(4-fluorophenyl)(phenyl)methyl]-1H-pyrrole-3-carbonitrile (13.7 g, 47.0 mmol) in ethanol (200 ml) was sequentially added acetylacetone (5.66 g, 56.6 mmol) and concentrated hydrochloric acid (2.0 ml). The mixture was heated under reflux for 3 hours, poured into saturated sodium bicarbonate solution and extracted with ethyl acetate. The extract was washed with water and dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. The residue was recrystallized from ethyl acetate and hexane.
WORKUP
后处理
- temperatureThe mixture was heated
- temperatureunder reflux for 3 hours
- extractionextracted with ethyl acetate
- washThe extract was washed with water
- dry with materialdried over anhydrous magnesium sulfate
- distillationthe solvent was distilled off under reduced pressure
- customThe residue was recrystallized from ethyl acetate and hexane