反应详情

温度

150 °C

6-Dimethylamino-2H-isoquinolin-1-one (50 mg, 0.27 mmol), Acetic acid 2,6-dibromo-benzyl ester (164 mg, 532 mmol), cuprous iodide (10 mg, 0.053 mmol), and potassium carbonate (37 mg, 0.27 mmol) were deposited in sealed vessel. 3 mL DMSO was added. Argon was bubbled through the mixture for 2 minutes and the lid was tightly closed. This was heated at 150° C. for 5 hours. The resulting mixture was partitioned between ethyl acetate and water. The organic layer was washed with brine, dried over anhydrous magnesium sulfate, concentrated in vacuo, and purified by flash chromatography (gradient elution 30 to 40% ethylacetate/hexanes) to yield Acetic acid 2-bromo-6-(6-dimethylamino-1-oxo-1H-isoquinolin-2-yl)-benzyl ester (48 mg, 0.12 mmol). MS (ESI) 417.0 (M+H)+.

1. customArgon was bubbled through the mixture for 2 minutes
2. customthe lid was tightly closed
3. customThe resulting mixture was partitioned between ethyl acetate and water
4. washThe organic layer was washed with brine
5. dry with materialdried over anhydrous magnesium sulfate
6. concentrationconcentrated in vacuo
7. custompurified by flash chromatography (gradient elution 30 to 40% ethylacetate/hexanes)