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Methanesulfonic Acid → HCID 178493039、化合物

HRID 1700597
ノート
印刷プレビュー

反応式

HRID 1700597 の反応式
[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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6395Methanesulfonic Acid2 回HCID 183177154-Methoxy-7-phenyl-5,6,7,8-tetrahydroquinolin-5-oneHCID 178418668HCID 178418668、化合物

生成物 1

HCID 178493039HCID 178493039、化合物収率 112.4%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
50 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-1691a1fd8bb54385a7c14bdb37ac3354
出典データセット
uspto-grants-2002_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06350749B1

反応ノート

読み込み中…

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