反应详情

To a solution of N-[6-(4-fluorobenzyl)-3-hydroxy-4-methoxy-5-oxo-5,6,7,8-tetrahydro-2,6-naphthyridin-1-yl]-N-methylmethanesulfonamide (0.0207 g, 0.506 mmol) in CH2Cl2 (6 mL) was added 30% by weight HBr in propionic acid (0.196 g HBr, 2.42 mmol). Alternatively, 30% HBr in acetic acid can be used. After 1.5 hours, the product mixture was evaporated and the residue partitioned between CHCl3 and 10% KHSO4. The organic extract was dried with Na2SO4, filtered, and concentrated under vacuum. The residual material was purified using reverse phase HPLC eluting with 5%-95% acetonitrile (0.1% TFA) in H2O (0.1% TFA) to afford the title compound.

1. customthe product mixture was evaporated
2. customthe residue partitioned between CHCl3 and 10% KHSO4
3. extractionThe organic extract
4. dry with materialwas dried with Na2SO4
5. filtrationfiltered
6. concentrationconcentrated under vacuum
7. customThe residual material was purified
8. washeluting with 5%-95% acetonitrile (0.1% TFA) in H2O (0.1% TFA)