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Sodium Hydroxide → N-[3-(7,8-Dimethoxy-1,3,4,5-tetrahydro-2H-3-benzazepin-2-on-3-yl)-propyl]-2-(3,4-dimethoxyphenylamino)-ethylamine

HRID 364073
ノート
印刷プレビュー

反応式

HRID 364073 の反応式
[CH3:1][O:2][C:3]1[C:18]([O:19][CH3:20])=[CH:17][C:6]2[CH2:7][C:8](=[O:16])[N:9]([CH2:12][CH2:13][CH2:14]Cl)[CH2:10][CH2:11][C:5]=2[CH:4]=1.[CH3:21][O:22][C:23]1[CH:24]=[C:25]([NH:31][CH2:32][CH2:33][NH2:34])[CH:26]=[CH:27][C:28]=1[O:29][CH3:30].[OH-].[Na+].C1(N)C(F)=C(F)C(F)=C(N)C=1F.Cl.Cl>C(Cl)Cl>[CH3:1][O:2][C:3]1[C:18]([O:19][CH3:20])=[CH:17][C:6]2[CH2:7][C:8](=[O:16])[N:9]([CH2:12][CH2:13][CH2:14][NH:34][CH2:33][CH2:32][NH:31][C:25]3[CH:26]=[CH:27][C:28]([O:29][CH3:30])=[C:23]([O:22][CH3:21])[CH:24]=3)[CH2:10][CH2:11][C:5]=2[CH:4]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 14798Sodium HydroxideHCID 149026Tetrafluoro-m-phenylenediamine dihydrochlorideHCID 130925103-(3-Chloropropyl)-7,8-dimethoxy-1,3,4,5-tetrahydro-2H-3-benzazepin-2-oneHCID 135796642-(3,4-Dimethoxyphenylamino)-ethylamine

生成物 1

HCID 13579665N-[3-(7,8-Dimethoxy-1,3,4,5-tetrahydro-2H-3-benzazepin-2-on-3-yl)-propyl]-2-(3,4-dimethoxyphenylamino)-ethylamine

試薬・触媒・溶媒

1
HCID 6344Dichloromethane溶媒

実験手順

Here, 3-(7,8-dimethoxy-1,3,4,5-tetrahydro-2H-3-benzazepin-2-on-3-yl)-1-chloropropane (10 g, 0.0336 mol) is heated to 130° C. for 3 hours with 2-(3,4-dimethoxyphenylamino)-ethylamine (13 g, 0.066 mol). After cooling, the reaction mixture is distributed between sodium hydroxide solution and methylene chloride. The organic phase is separated, dried over sodium sulfate and concentrated. The residue is chromatographed on silica gel (eluant: methylene chloride/methanol/conc. ammonia: 90/10/0.25). The product thus obtained is converted into the dihydrochloride in the usual way.

後処理

  1. temperatureAfter cooling
  2. customThe organic phase is separated
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated
  5. customThe residue is chromatographed on silica gel (eluant: methylene chloride/methanol/conc. ammonia: 90/10/0.25)
  6. customThe product thus obtained

出典と根拠

ORDレコード
ord-5ace4c2822404296ac4ec664c4654068
出典データセット
uspto-grants-1986_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04604389

反応ノート

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