反应详情

温度

60 °C

N-(3-(3-Methoxy-5-nitrophenylamino)quinoxalin-2-yl)-3-nitrobenzenesulfonamide (400 mg, 0.81 mmol), prepared as described above in Example 115, was dissolved in 1:1 THF:EtOH (4 mL), to which was added formic acid (938 μl, 2.42 mmol) and potassium formate (203 mg, 2.42 mmol). The system was flushed with nitrogen, and then 10% wt Pd/C (50 mg) was added. The reaction was then heated to 60° C. Once the reaction was determined complete by LC-MS, it was allowed to cool, and DMF was added for solubility. The solution was then filtered through a nylon fit to remove the catalyst. The filtrate was diluted water and the pH adjusted to 7 and extracted with DCM (2×) and EtOAc (2×). All organic layers were combined and evaporated to dryness to give 3-amino-N-(3-(3-amino-5-methoxyphenylamino)quinoxalin-2-yl)benzenesulfonamide (330 mg, 93%). MS (EI) m/z for C21H20N6O3S: 437.06 (MH+)

1. customThe system was flushed with nitrogen
2. addition10% wt Pd/C (50 mg) was added
3. temperatureto cool
4. additionDMF was added for solubility
5. filtrationThe solution was then filtered through a nylon
6. customto remove the catalyst
7. extractionextracted with DCM (2×) and EtOAc (2×)
8. customevaporated to dryness