反应详情

7-Methyl-2H-isoquinolin-1-one (2.1 g, 13.2 mmol) in phosphorus oxychloride (30 mL) is heated to reflux for 13 hours. The mixture is cooled to room temperature, then concentrated to a smaller volume. The residue is diluted with ice water and the pH is adjusted to ca. 8 by slow addition of 10 N NaOH. The aqueous solution is extracted with methylene chloride (4×20 mL) and the combined organic layers are washed with brine, dried over MgSO4, filtered and concentrated. The resulting dark oil is purified by column chromatography eluting with 25% EtOAc/hexanes to give the product (1.6 g, 9 mmol) as a light yellow solid.

1. temperatureto reflux for 13 hours
2. concentrationconcentrated to a smaller volume
3. additionThe residue is diluted with ice water
4. additionby slow addition of 10 N NaOH
5. extractionThe aqueous solution is extracted with methylene chloride (4×20 mL)
6. washthe combined organic layers are washed with brine
7. dry with materialdried over MgSO4
8. filtrationfiltered
9. concentrationconcentrated
10. customThe resulting dark oil is purified by column chromatography
11. washeluting with 25% EtOAc/hexanes