Nitric Acid → Acea-1416

HRID 1857446노트

반응식

HRID 1857446 반응식
[Cl:1][C:2]1[CH:11]=[C:10]2[C:5]([NH:6][CH2:7][C:8](=[O:12])[NH:9]2)=[CH:4][C:3]=1[CH3:13].[N+:14]([O-])([OH:16])=[O:15].C(O)(C(F)(F)F)=[O:19]>>[Cl:1][C:2]1[CH:11]=[C:10]2[C:5]([NH:6][C:7](=[O:19])[C:8](=[O:12])[NH:9]2)=[C:4]([N+:14]([O-:16])=[O:15])[C:3]=1[CH3:13]

참가 물질

4

반응물 3

HCID 944Nitric AcidHCID 6422Trifluoroacetic acidHCID 100814077-Chloro-3,4-dihydro-6-methyl-2(1H)-quinoxalinone

생성물 1

HCID 9816526Acea-1416

실험 절차

To a stirred suspension of 7-chloro-3,4-Dihydro-6-methyl-quinoxaline-2(1H)-one (0.100 g, 0.51 mmol) in TFA (3.0 mL) prepared as in Example 8, excess fuming HNO3 (0.30 mL) was added and the resulting red solution was stirred overnight at room temperature. The solvent was removed under vacuum and the residue diluted with water (4.0 mL). The precipitated solid was filtered and dried under vacuum to yield 0.067 g (52%) pure (HPLC) title compound as a light yellow powder; mp-darkens at 340° C.; 1H NMR (DMSO-d6) δ 2.184 (s, 3H), 7.263 (s, 1H), 11.948 (s, 1H), 12.144 (s, 1H); Anal for C9H6CIN3O4 ·H2O calcd C, 40.85; H, 2.28; N, 15.87, found C, 40.63; H, 2.05; N, 15.75.

후처리

  1. additionwas added
  2. customThe solvent was removed under vacuum
  3. additionthe residue diluted with water (4.0 mL)
  4. filtrationThe precipitated solid was filtered
  5. customdried under vacuum

출처 및 근거

ORD 기록
ord-24c6b472157e4aedb21db5dcde180dc6
출처 데이터셋
uspto-grants-2000_11
특허 번호
US06147075

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