反应详情

To a flask containing 2-tert-butyl 3-methyl 8-bromo-4-oxo-3,4-dihydroisoquinoline-2,3(1H)-dicarboxylate (24-1) (3.44 g, 8.95 mmol) (mixed with impurities) was added was added Dioxane (20 ml), then 5N HCl in H2O (20 ml, 100 mmol). The reaction mixture was then heated to 90 C in the hood overnight. Followed by LC/MS. The next morning another 20 mL of 5N HCl was added and the reaction mixture was heated to 110 C for 3 hours, then was concentrated. The resulting residue was triturated with DCM (hot, then cooled to room temperature) & filtered to yield 8-bromo-2,3-dihydroisoquinolin-4(1H)-one hydrochloride (24-2). HRMS [M+H]: calculated; 225.9862, observed; 225.9860.

1. additionwas added
2. temperatureThe reaction mixture was then heated to 90 C in the hood overnight
3. temperaturethe reaction mixture was heated to 110 C for 3 hours
4. concentrationwas concentrated
5. customThe resulting residue was triturated with DCM (hot,
6. filtrationfiltered