反应详情

Methyl 8-(benzyloxy)-5-bromo-1,6-naphthyridine-7-carboxylate (Example 1; 5.50 g; 14.7 mmol) was dissolved in DMA (300 ml). DIPEA (5.14 ml; 29.5 mmol) was added at room temperature. The reaction mixture was stirred for 5 min at room temperature. tert-Butyl 6-aminohexylcarbamate (4.95 ml; 22.1 mmol) was added and the reaction mixture was stirred at 100° C. for 12 hours. The reaction mixture was cooled. Water and ethyl acetate were added. The organic layer was separated and washed with water (×2) and with brine. The organic layer was dried (MgSO4), filtered and the solvent was evaporated. The residue was purified by flash column chromatography over silica gel (eluent: hexane/EtOAc from 10:1 to 1:1). The product fractions were collected and the solvent evaporated.

1. stirringthe reaction mixture was stirred at 100° C. for 12 hours
2. temperatureThe reaction mixture was cooled
3. customThe organic layer was separated
4. washwashed with water (×2) and with brine
5. dry with materialThe organic layer was dried (MgSO4)
6. filtrationfiltered
7. customthe solvent was evaporated
8. customThe residue was purified by flash column chromatography over silica gel (eluent: hexane/EtOAc from 10:1 to 1:1)
9. customThe product fractions were collected
10. customthe solvent evaporated