반응 #532721

반응 방정식

6-bromo-4-chloro-3-nitro-quinoline

4-amino-1,3-dimethylpyrazole

HCl

1,2,2,6,6-pentamethylpiperidine

→

title compound

(6-Bromo-3-nitro-quinolin-4-yl)-(1,3-dimethyl-1H-pyrazol-4-yl)-amine

용매

DMA

반응 조건

후처리

1. 1
   온도Then the RM was cooled down to rt
2. 2
   기타quenched with H2O
3. 3
   여과The suspension was filtered
4. 4
   세척the solid cake was washed with H2O
5. 5
   기타dried under vacuum
6. 6
   workup.DISSOLUTIONbefore being dissolved in EtOAc
7. 7
   세척The solution was washed with brine (2×)
8. 8
   건조dried over Na2SO4
9. 9
   여과filtered
10. 10
    기타evaporated to dryness

실험 절차

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)

출처