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Ammonia → HCID 19990453, 화합물

HRID 346129
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HRID 346129 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([N+:20]([O-:22])=O)[C:5]([NH:12][C:13]([C:15](OCC)=[O:16])=[O:14])=[C:6]([C:8]([F:11])([F:10])[F:9])[CH:7]=1.CN(C)C=O.N.[H][H]>O1CCCC1.[Pt]>[Cl:1][C:2]1[CH:3]=[C:4]2[C:5]([NH:12][C:13](=[O:14])[C:15](=[O:16])[N:20]2[OH:22])=[C:6]([C:8]([F:11])([F:10])[F:9])[CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 222AmmoniaHCID 6228DimethylformamideHCID 199803055-Chloro-2-ethoxalylamino-3-nitrobenzotrifluorideHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 19990453HCID 19990453, 화합물수율 80%

시약·촉매·용매 2

HCID 23939Platinum촉매
HCID 8028
Tetrahydrofuran
용매

실험 절차

To a solution of 1.0 g (2.94 mmol) 5-chloro-2-ethoxalylamino-3-nitrobenzotrifluoride in 75 ml tetrahydrofuran was added 25 ml dimethylformamide and 1.0 ml 25% aqueous ammonia. The mixture was hydrogenated at atm. pressure by using 100 mg 5% Pt-C as a catalyst. When the hydrogen uptake was completed, the catalyst was filtered off, and the filtrate was evaporated in vacuo. The residue was stirred with 1N aqueous hydrochloric acid to give 0.66 g (80%) of 7-chloro-1-hydroxy-5-trifluoromethylquinoxaline -2,3(1H,4H)-dione. M.P. 275° C. decomp. 1H-NMR (DMSO-d6): 11.7 (2H, m), 7.60 (1H, d), 7.43 (1H, d).

후처리

  1. filtrationthe catalyst was filtered off
  2. customthe filtrate was evaporated in vacuo

출처 및 근거

ORD 기록
ord-bad14492cfd64b5abb46796909190fec
출처 데이터셋
uspto-grants-1991_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05061706

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