反应详情

To a solution of 1-amino-6-fluoro-isoquinoline (0.41 g, 2.53 mmol) in CHCl3 (25 mL) is added NBS (0.45 g, 2.53 mmol), and the reaction mixture is stirred RT for 1.5 h. The reaction mixture is treated with water (10 mL). The aqueous phase is extracted with CH2Cl2 (2×). The combined organic layers are washed with brine, and dried over MgSO4. The solvent is evaporated and the residue is dried under vacuum. Purification of the crude material using a Biotage column (10-40% MeOH/CH2Cl2) afforded 0.395 g (65%) of 1-amino-4-bromo-6-fluoro-isoquinoline. LC/MS m/z=242 [M+H]+.

1. extractionThe aqueous phase is extracted with CH2Cl2 (2×)
2. washThe combined organic layers are washed with brine
3. dry with materialdried over MgSO4
4. customThe solvent is evaporated
5. customthe residue is dried under vacuum
6. customPurification of the crude material