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Methanesulfonic Acid → HCID 178493039, 화합물

HRID 1700597
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인쇄 미리보기

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HRID 1700597 반응식
[C:1]([NH:4][NH2:5])([NH2:3])=[NH:2].Cl.[CH3:7][S:8]([OH:11])(=[O:10])=[O:9].[CH3:12][O:13][C:14]1[C:23]2[C:22](=O)[CH2:21][CH:20]([C:25]3[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=3)[CH2:19][C:18]=2[N:17]=[CH:16][CH:15]=1>C(O)C>[CH3:7][S:8]([OH:11])(=[O:10])=[O:9].[NH:4]([N:5]=[C:22]1[CH2:21][CH:20]([C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)[CH2:19][C:18]2[N:17]=[CH:16][CH:15]=[C:14]([O:13][CH3:12])[C:23]1=2)[C:1]([NH2:3])=[NH:2]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6395Methanesulfonic Acid2회HCID 183177154-Methoxy-7-phenyl-5,6,7,8-tetrahydroquinolin-5-oneHCID 178418668HCID 178418668, 화합물

생성물 1

HCID 178493039HCID 178493039, 화합물수율 112.4%

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
50 °C

실험 절차

To a solution of aminoguanidine hydrochloride (0.023 g) in ethanol (10 ml) was added methanesulfonic acid (0.02 g), and the mixture was refluxed for 30 minutes. To the solution was added 4-methoxy-7-phenyl-5,6,7,8-tetrahydroquinolin-5-one (0.05 g), and the mixture was stirred at room temperature for 2 hours and 20 minutes and at 50° C. for 25 minutes. To the mixture was added methanesulfonic acid (0.02 g), and the mixture was stirred at 50° C. for 5 hours. Under reduced pressure, the solvent was evaporated, and the residue was dissolved in water. The solution was washed with ethyl acetate. Under reduced pressure, the solvent was evaporated, and the residue was recrystallized from ethanol-water to give 5-guanidinoimino-4-methoxy-7-phenyl-5,6,7,8-tetrahydroquinoline methanesulfonate (Compound 78) (0.09 g) as colorless crystals.

후처리

  1. temperaturethe mixture was refluxed for 30 minutes
  2. stirringthe mixture was stirred at 50° C. for 5 hours
  3. customUnder reduced pressure, the solvent was evaporated
  4. dissolutionthe residue was dissolved in water
  5. washThe solution was washed with ethyl acetate
  6. customUnder reduced pressure, the solvent was evaporated
  7. customthe residue was recrystallized from ethanol-water

출처 및 근거

ORD 기록
ord-1691a1fd8bb54385a7c14bdb37ac3354
출처 데이터셋
uspto-grants-2002_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06350749B1

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