HRID2183551
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
A mixture of 3-amino-1-methyl-4-(2,4,6-trimethylphenyl)-1H-pyrrole-2-carbonitrile (2 mmol), methyl acetoacetate (4 mmol) and SnCl4 (4 mmol) in 1,2-dichloroethane was heated at reflux for about six hours until all the starting material were consumed. The mixture was quenched with acetone, basified with saturated NaHCO3, then filtered through Celite?. The filtrate was concentrated to dryness. The residue was quenched with water and extracted with chloroform. The chloroform layer was washed with brine, dried and concentrated to dryness to give 7-amino-1,5-dimethyl-3-(2,4,6-trimethyl-phenyl)-1H-pyrrolo[3,2-b]pyridine-6-carboxylic acid methyl ester. The product may be purified by trituration.
WORKUP
后处理
- temperaturewas heated
- temperatureat reflux for about six hours until all the starting material
- customwere consumed
- customThe mixture was quenched with acetone
- filtrationfiltered through Celite
- concentrationThe filtrate was concentrated to dryness
- customThe residue was quenched with water
- extractionextracted with chloroform
- washThe chloroform layer was washed with brine
- customdried
- concentrationconcentrated to dryness