تفاعل #532721

معادلة التفاعل

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

المذيبات

DMA

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةThen the RM was cooled down to rt
2. 2
   أخرىquenched with H2O
3. 3
   ترشيحThe suspension was filtered
4. 4
   غسيلthe solid cake was washed with H2O
5. 5
   أخرىdried under vacuum
6. 6
   workup.DISSOLUTIONbefore being dissolved in EtOAc
7. 7
   غسيلThe solution was washed with brine (2×)
8. 8
   تجفيفdried over Na2SO4
9. 9
   ترشيحfiltered
10. 10
    أخرىevaporated to dryness

الإجراء التجريبي

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)

المصدر