反应详情

1-Cyclopropyl-5-hydroxy-isoquinoline-7-carboxylic acid methyl ester (5.00 g, 20.6 mmol) was dissolved in DMF (50 ml) and K2CO3 (5.69 g, 41.2 mmol) and MeI (1.54 ml, 24.7 mmol) was added thereto. After stirred at room temperature for 2 h, the reaction mixture was diluted with EtOAc and H2O. The aqueous layer was extracted with EtOAc and the organic layer was washed with brine, dried over MgSO4. The desiccant was removed through filtration and the filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (hexane/EtOAc=10/0 to 6/4) to obtain the intended compound as a colorless solid.

1. extractionThe aqueous layer was extracted with EtOAc
2. washthe organic layer was washed with brine
3. dry with materialdried over MgSO4
4. customThe desiccant was removed through filtration
5. concentrationthe filtrate was concentrated under reduced pressure
6. customThe residue was purified by silica gel column chromatography (hexane/EtOAc=10/0 to 6/4)