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Water → TAK-603

HRID 1458925
ノート
印刷プレビュー

反応式

HRID 1458925 の反応式
[H-].[Na+].[NH:3]1[CH:7]=[N:6][CH:5]=[N:4]1.Cl[CH2:9][C:10]1[C:19]([C:20]([O:22][CH2:23][CH3:24])=[O:21])=[C:18]([C:25]2[CH:30]=[CH:29][C:28]([O:31][CH3:32])=[C:27]([O:33][CH3:34])[CH:26]=2)[C:17]2[C:12](=[CH:13][C:14]([O:37][CH3:38])=[C:15]([O:35][CH3:36])[CH:16]=2)[N:11]=1.O>CN(C)C=O>[CH3:36][O:35][C:15]1[CH:16]=[C:17]2[C:12](=[CH:13][C:14]=1[O:37][CH3:38])[N:11]=[C:10]([CH2:9][N:3]1[CH:7]=[N:6][CH:5]=[N:4]1)[C:19]([C:20]([O:22][CH2:23][CH3:24])=[O:21])=[C:18]2[C:25]1[CH:30]=[CH:29][C:28]([O:31][CH3:32])=[C:27]([O:33][CH3:34])[CH:26]=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 962WaterHCID 92571H-1,2,4-TriazoleHCID 24758Sodium hydrideHCID 10813243Ethyl 2-chloromethyl-4-(3,4-dimethoxyphenyl)-6,7-dimethoxyquinoline-3-carboxylate

生成物 1

HCID 153980TAK-603収率 53%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide
溶媒

実験手順

Oily sodium hydride (60%, 0.323 g) was added to a solution of 1H-1,2,4-triazole (0.558 g) in N,N-dimethylformamide (30 ml), and the mixture was stirred at room temperature for 15 minutes. Then ethyl 2-chloromethyl-6,7-dimethoxy-4-(3,4-dimethoxyphenyl)quinoline-3-carboxylate(3.0 g) was added. The mixture was stirred at 80° C. for 1 hour, poured into water and extracted with ethyl acetate. The ethyl acetate layer was washed with water and dried over magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was subjected to column chromatography on silica gel. The fractions firstly eluted with chloroform/methanol (40/1, v/v) gave ethyl 6,7-dimethoxy-4-(3,4-dimethoxyphenyl)-2-(1,2,4-triazol-1-ylmethyl)quinoline-3-carboxylate (1.7 g, 53%) which was then recrystallized from ethyl acetate-hexane. Colorless prisms. mp. 176°-177° C.

後処理

  1. stirringThe mixture was stirred at 80° C. for 1 hour
  2. extractionextracted with ethyl acetate
  3. washThe ethyl acetate layer was washed with water
  4. dry with materialdried over magnesium sulfate
  5. customthe solvent was evaporated under reduced pressure
  6. washThe fractions firstly eluted with chloroform/methanol (40/1

出典と根拠

ORDレコード
ord-aea9c2558d1347119a4e435878f0d32e
出典データセット
uspto-grants-1998_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05852039

反応ノート

読み込み中…

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