HRID730415
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 2-amino-1-(indan-1-yl)pyrrole-4-carbonitrile (19.4 g), acetylacetone (9.6 g) and ethanol (375 ml) was added concentrated hydrochloric acid (3 ml), and the mixture was heated under reflux for 3 hours. The reaction solution was concentrated under reduced pressure and an aqueous sodium hydrogen carbonate solution was added to the residue, which was extracted with ethyl acetate. After the organic layer was washed with water and dried (MgSO4), the solvent was distilled off under reduced pressure and the crystal was collected by filtration to give 1-(indan-1-yl)-4,6-dimethyl-1H-pyrrolo[2,3-b]pyridine-3-carbonitrile (11.4 g, 46%).
WORKUP
后处理
- temperaturethe mixture was heated
- temperatureunder reflux for 3 hours
- concentrationThe reaction solution was concentrated under reduced pressure
- additionan aqueous sodium hydrogen carbonate solution was added to the residue, which
- extractionwas extracted with ethyl acetate
- washAfter the organic layer was washed with water
- dry with materialdried (MgSO4)
- distillationthe solvent was distilled off under reduced pressure
- filtrationthe crystal was collected by filtration