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Methylamine → HCID 69961311, 화합물

HRID 369269
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HRID 369269 반응식
[Cl:1][C:2]1[C:3](F)=[C:4]([F:27])[CH:5]=[C:6]2[C:11]=1[N:10]([C:12]1[CH:17]=[C:16]([OH:18])[C:15]([F:19])=[CH:14][C:13]=1[N+:20]([O-:22])=[O:21])[CH:9]=[C:8]([C:23]([OH:25])=[O:24])[C:7]2=[O:26].[CH3:29][NH2:30]>>[CH3:9][NH2:10].[Cl:1][C:2]1[C:3]([NH:30][CH3:29])=[C:4]([F:27])[CH:5]=[C:6]2[C:11]=1[N:10]([C:12]1[CH:17]=[C:16]([OH:18])[C:15]([F:19])=[CH:14][C:13]=1[N+:20]([O-:22])=[O:21])[CH:9]=[C:8]([C:23]([OH:25])=[O:24])[C:7]2=[O:26]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 6329MethylamineHCID 23284711HCID 23284711, 화합물

생성물 1

HCID 69961311HCID 69961311, 화합물수율 145.3%

실험 절차

8-Chloro-6,7-difluoro-1-(4-fluoro-5-hydroxy-2-nitrophenyl)-4-oxo-1,4-dihydroquinoline-3-carboxylic acid (150 mg) was added to an aqueous solution (about 40%; 750 mg) of methylamine, and the mixture was stirred at room temperature for 6 hours. The reaction mixture was concentrated under reduced pressure. A process of adding ethanol (2 ml) to the residue and then concentrating the mixture under reduced pressure was conducted 3 times repeatedly. Isopropyl alcohol (1.5 ml) was added to the resultant residue. Deposits were collected by filtration and washed with isopropyl alcohol and diisopropyl ether in that order to obtain the title compound (120 mg) as a yellow powder.

후처리

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. concentration
A process of adding ethanol (2 ml) to the residue and then concentrating the mixture under reduced pressure
  • additionIsopropyl alcohol (1.5 ml) was added to the resultant residue
  • filtrationDeposits were collected by filtration
  • washwashed with isopropyl alcohol and diisopropyl ether in that order
  • 출처 및 근거

    ORD 기록
    ord-469cdb08424041e28c944958927f0117
    출처 데이터셋
    uspto-grants-2000_10
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US06136823

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