反应详情

Sodium hydride (2.2 equiv., 0.844 mmol, 0.034 g (60%)) was added to a solution of tert-butyl cyanoacetate (1.2 equiv., 0.460 mmol, 0.065 g) in dry pyridine (1 ml) under Ar atmosphere. The catalyst—prepared as described above—was injected, and the mixture was stirred at room temperature for 5 min. Compound 21 (1.0 equiv., 0.383 mmol, 0.150 g) was then added and the reaction mixture was heated at 85° C. for 2 h. After destruction of excess sodium hydride with methanol, the solvent was concentrated under vacuum. The residue was purified by column chromatography (dichloromethane/methanol (7M NH3) 95:5) to give dimethylethyl 5-[5,6-dihydro-5-oxo-pyrido[2′,1′:2,3]imidazo[4,5-c]isoquinolin-6-yl]-α-cyano-2-pyridineacetate (I12) (0.078 g, yield=45%).

1. customThe catalyst—prepared
2. temperaturethe reaction mixture was heated at 85° C. for 2 h
3. customAfter destruction of excess sodium hydride with methanol
4. concentrationthe solvent was concentrated under vacuum
5. customThe residue was purified by column chromatography (dichloromethane/methanol (7M NH3) 95:5)