Nitric Acid → 6-Bromo-7-chloro-5-nitroquinoxaline-2(1H)-one

HRID 1068608노트

반응식

HRID 1068608 반응식
[Br:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][C:11]=1[Cl:12])[NH:8][C:7](=[O:13])[CH2:6][NH:5]2.[N+:14]([O-])([OH:16])=[O:15]>C(O)(C(F)(F)F)=O>[Br:1][C:2]1[C:3]([N+:14]([O-:16])=[O:15])=[C:4]2[C:9](=[CH:10][C:11]=1[Cl:12])[NH:8][C:7](=[O:13])[CH:6]=[N:5]2

참가 물질

4

반응물 2

HCID 944Nitric AcidHCID 100383166-bromo-7-chloro-3,4-dihydroquinoxalin-2(1H)-one

생성물 1

HCID 211899856-Bromo-7-chloro-5-nitroquinoxaline-2(1H)-one수율 70%

시약·촉매·용매 1

HCID 6422Trifluoroacetic acid용매

실험 절차

To a stirred suspension of 6-bromo-7-chloro-3,4-dihydroquinoxaline-2(1H)-one (0.06 g, 0.23 mmol, as obtained above) in CF3COOH (0.5 mL) was added fuming HNO3 (0.02 mL, 0.46 mmol) and the resulting reddish yellow suspension was stirred at room temperature overnight The cream colored suspension so obtained was poured into ice (2.5 mL) and the precipitated solid was filtered, washed with water (1.0 mL), and dried under vacuum to afford 0.049 g (70%) of the title compound as a cream colored powder. 1H NMR (DMSO-d6): δ 7.577 (s, 1H), 8.251 (s, 1H), 12.879 (s, 1H). The crude product was used as such for the final reaction.

후처리

  1. customso obtained
  2. filtrationthe precipitated solid was filtered
  3. washwashed with water (1.0 mL)
  4. customdried under vacuum

출처 및 근거

ORD 기록
ord-98544b832cc34fe1b3820743489efef5
출처 데이터셋
uspto-grants-2001_06
특허 번호
US06251903B1

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