反应详情

温度

135 °C

Into a pressure reactor was placed 5-bromo-N-(2,3-dimethoxybenzyl)-8-hydroxy-1,6-naphthyridine-7-carboxamide (0.1 g, 0.24 mmol), 4-(dimethylamino)benzenethiol (0.147 g, 0.96 mmol) and triethylamine (0.363 g, 0.5 mL, 3.59 mmol). The vessel was purged with nitrogen gas, sealed and heated to 135° C. for 18 hours, after which time it was cooled and the excess triethylamine removed in vacuo. The residue was partitioned between EtOAc/water and extracted. The combined organic extracts were washed with brine, dried over Na2SO4, filtered and the solvent removed. The resulting glass was triturated with diethyl ether and filtered to yield N-(2,3-dimethoxybenzyl)-5-{[4-(dimethylamino)phenyl]thio}-8-hydroxy-1,6-naphthyridine-7-carboxamide as a solid.

1. customInto a pressure reactor was placed
2. customThe vessel was purged with nitrogen gas
3. customsealed
4. temperatureafter which time it was cooled
5. customthe excess triethylamine removed in vacuo
6. customThe residue was partitioned between EtOAc/water
7. extractionextracted
8. washThe combined organic extracts were washed with brine
9. dry with materialdried over Na2SO4
10. filtrationfiltered
11. customthe solvent removed
12. customThe resulting glass was triturated with diethyl ether
13. filtrationfiltered