反应详情

To the obtained (−)-3-(pyrrolidin-3-yl)-5-methyl-2H-isoquinolin-1-one (3.0 g) were added bromoethanol (8.21 g), sodium hydrogen carbonate (5.6 g), methyl ethyl ketone (84 ml) and water (8.4 ml), and the mixture was stirred under reflux for 2 hr. The reaction mixture was concentrated, extracted with methylene chloride, and the extract was washed with water, dried over magnesium sulfate and concentrated. The obtained residue was purified by column chromatography (methanol/ethyl acetate; 2/5) and crystallized from ethyl acetate to give (−)-3-[1-(2-hydroxylethyl)pyrrolidin-3-yl]-5-methyl-2H-isoquinolin-1-one (1.5425 g).

1. temperatureunder reflux for 2 hr
2. concentrationThe reaction mixture was concentrated
3. extractionextracted with methylene chloride
4. washthe extract was washed with water
5. dry with materialdried over magnesium sulfate
6. concentrationconcentrated
7. customThe obtained residue was purified by column chromatography (methanol/ethyl acetate; 2/5)
8. customcrystallized from ethyl acetate