反应详情

To a mixture of 6-Bromo-isoquinolin-1-ylamine (0.80 g), Boc-L-proline (0.803 g), and 4-methylmorpholine (0.83 mL) in DMF (10 mL) was added HATU (1.39 g). Reaction mixture was stirred for 6 hours. Additional Boc-L-proline (0.803 g), 4-methylmorpholine (0.83 mL) and HATU (1.39 g) were added and reaction stirred overnight at ambient temperature and then concentrated. The residue was dissolved in ethyl acetate and washed with 10:1 H2O/saturated sodium bicarbonate solution, 5% lithium chloride solution, brine and dried (MgSO4), concentrated and purified by flash column chromatography (silica gel, 20 to 70% ethyl acetate/hexanes) to give 2-(6-Bromo-isoquinolin-1-yl carbamoyl)-pyrrolidine-1-carboxylic acid tert-butyl ester (1.74 g): LCMS-ESI+: calc'd for C19H23BrN3O3: 421.31 (M+H+); Found: 419.8, 421.8 (M+H+).

1. customReaction mixture
2. customreaction
3. stirringstirred overnight at ambient temperature
4. concentrationconcentrated
5. dissolutionThe residue was dissolved in ethyl acetate
6. washwashed with 10:1 H2O/saturated sodium bicarbonate solution, 5% lithium chloride solution, brine
7. dry with materialdried (MgSO4)
8. concentrationconcentrated
9. custompurified by flash column chromatography (silica gel, 20 to 70% ethyl acetate/hexanes)