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 ethyl 2-bromomethyl-4-(3-nitrophenyl)-6-phenyl-3-pyridinecarboxylate (1.5 g) and 2-dimethylaminoethylamine (0.6 g) in isopropyl alcohol (15 ml) was refluxed for 1 hour. The reaction mixture was evaporated in vacuo and the residue was dissolved in a mixture of water (20 ml) and chloroform (40 ml). The organic layer was washed with water and dried over magnesium sulfate. The solvent was distilled off. The residue was subjected to a column chromatography on silica gel, eluting with a mixture of chloroform and methanol (50:1 V/V). The fractions containing the desired compound were combined and evaporated in vacuo. The crystalline residue was recrystallized from ethanol to give 6-(2-dimethylaminoethyl)-4-(3-nitrophenyl)-5-oxo- 2-phenyl-5,7-dihydro-(6H)-pyrrolo[3,4-b]pyridine (0.49 g).
WORKUP
后处理
- temperaturewas refluxed for 1 hour
- customThe reaction mixture was evaporated in vacuo
- dissolutionthe residue was dissolved in a mixture of water (20 ml) and chloroform (40 ml)
- washThe organic layer was washed with water
- dry with materialdried over magnesium sulfate
- distillationThe solvent was distilled off
- washeluting with a mixture of chloroform and methanol (50:1 V/V)
- additionThe fractions containing the desired compound
- customevaporated in vacuo
- customThe crystalline residue was recrystallized from ethanol