反应详情

温度

50 °C

To a mixture of 6-bromo-4-chloro-3-nitro-quinoline (Stage A.4, 3.0 g, 20.43 mmol) and 4-amino-1,3-dimethylpyrazole.HCl (ChemCollect, Remscheid, Germany, 1.85 g, 12.53 mmol) in DMA (45 ml) was added 1,2,2,6,6-pentamethylpiperidine (6.67 ml, 36.5 mmol). The RM was stirred at 50° C. for 4.5 h. Then the RM was cooled down to rt and quenched with H2O. The suspension was filtered, the solid cake was washed with H2O and dried under vacuum, before being dissolved in EtOAc. The solution was washed with brine (2×), dried over Na2SO4, filtered and evaporated to dryness to give the title compound as an orange solid (HPLC tR 2.55 min (Method A); M+H=362; M−H=360 MS-ES)

1. temperatureThen the RM was cooled down to rt
2. customquenched with H2O
3. filtrationThe suspension was filtered
4. washthe solid cake was washed with H2O
5. customdried under vacuum
6. dissolutionbefore being dissolved in EtOAc
7. washThe solution was washed with brine (2×)
8. dry with materialdried over Na2SO4
9. filtrationfiltered
10. customevaporated to dryness