반응 #82661

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5,6,7-trifluoro-1,4-dihydro-2,3-quinoxalinedione

sulfuric acid

KNO3

→

5-Nitro-6,7,8-trifluoro-1,4-dihydro-2,3-quinoxalinedione

반응 조건

후처리

1. 1
   기타giving a brown mixture, which
2. 2
   기타instantly giving an orange precipitate, which
3. 3
   기타is collected by centrifugation
4. 4
   기타The powder was crystallized from EtOH (5 mL)
5. 5
   기타dried in vacuo
6. 6
   기타to yield 24 mg (20%) of pale orange microcrystals

실험 절차

To 5,6,7-trifluoro-1,4-dihydro-2,3-quinoxalinedione (93 mg, 0.43 mmol) is added concentrated sulfuric acid (0.5 mL). While the flask is an ice bath, KNO3 is slowly added, giving a brown mixture, which is stirred overnight. The reaction mixture, now dark red, is then added into ice water (5 mL), instantly giving an orange precipitate, which is collected by centrifugation. The powder was crystallized from EtOH (5 mL) and dried in vacuo to yield 24 mg (20%) of pale orange microcrystals. 1H NMR (DMSO-d6), 11.9 (br s, 1H), 12.6 (br s, 1H).

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