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Hydrochloric Acid → HCID 10647202、化合物

HRID 1648271
ノート
印刷プレビュー

反応式

HRID 1648271 の反応式
C([O:3][C:4]([C:6]1[C:7]([CH2:30][N:31]2[CH:35]=[N:34][CH:33]=[N:32]2)=[N:8][C:9]2[C:14]([C:15]=1[C:16]1[CH:21]=[CH:20][C:19]([O:22][CH3:23])=[C:18]([O:24][CH3:25])[CH:17]=1)=[CH:13][C:12]([O:26][CH3:27])=[C:11]([O:28][CH3:29])[CH:10]=2)=[O:5])C.[OH-].[Na+].Cl>C(O)C>[CH3:27][O:26][C:12]1[CH:13]=[C:14]2[C:9](=[CH:10][C:11]=1[O:28][CH3:29])[N:8]=[C:7]([CH2:30][N:31]1[CH:35]=[N:34][CH:33]=[N:32]1)[C:6]([C:4]([OH:5])=[O:3])=[C:15]2[C:16]1[CH:21]=[CH:20][C:19]([O:22][CH3:23])=[C:18]([O:24][CH3:25])[CH:17]=1
参加物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 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 153980TAK-603

生成物 1

HCID 10647202HCID 10647202、化合物収率 46%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 6,7-dimethoxy-4-(3,4-dimethoxyphenyl)-2-(1,2,4-triazol-1-ylmethyl)quinoline-3-carboxylic acid ethyl ester (3.0 g), 2N sodium hydroxide (15.6 ml) and ethanol (50 ml) was stirred under refluxing conditions for 8 hours. The reaction mixture was cooled with ice and adjusted to pH 5 with 2N hydrochloric acid, after which it was concentrated under reduced pressure. The residue was dissolved in ethanol, and the insoluble substances were filtered off. After the filtrate was concentrated, the residual oily substance was subjected to silica gel column chromatography and eluted with chloroform-methanol (4:1, v/v) to yield 6,7-dimethoxy-4-(3,4-dimethoxyphenyl)-2-(1,2,4-triazol- 1-ylmethyl)quinoline-3-carboxylic acid (1.3 g, 46%), which was then recrystallized from dichloromethane-ethanol to yield a colorless prismatic crystal having a melting point of 270° to 271° C. (decomposed).

後処理

  1. temperatureThe reaction mixture was cooled with ice
  2. concentrationafter which it was concentrated under reduced pressure
  3. dissolutionThe residue was dissolved in ethanol
  4. filtrationthe insoluble substances were filtered off
  5. concentrationAfter the filtrate was concentrated
  6. washeluted with chloroform-methanol (4:1

出典と根拠

ORDレコード
ord-70535f60efca4034b2d804a9621fab04
出典データセット
uspto-grants-1995_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05436247

反応ノート

読み込み中…

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