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Water → 2-(4-Fluoroanilino)-4-(isoquinolin-4-yl)benzoic acid

HRID 2191661
ノート
印刷プレビュー

反応式

HRID 2191661 の反応式
FC(F)(F)C(O)=O.[F:8][C:9]1[CH:38]=[CH:37][C:12]([NH:13][C:14]2[CH:26]=[C:25]([C:27]3[C:36]4[C:31](=[CH:32][CH:33]=[CH:34][CH:35]=4)[CH:30]=[N:29][CH:28]=3)[CH:24]=[CH:23][C:15]=2[C:16]([O:18]C(C)(C)C)=[O:17])=[CH:11][CH:10]=1.O.[OH-].[Na+]>C(OCC)(=O)C>[F:8][C:9]1[CH:38]=[CH:37][C:12]([NH:13][C:14]2[CH:26]=[C:25]([C:27]3[C:36]4[C:31](=[CH:32][CH:33]=[CH:34][CH:35]=4)[CH:30]=[N:29][CH:28]=3)[CH:24]=[CH:23][C:15]=2[C:16]([OH:18])=[O:17])=[CH:11][CH:10]=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 6422Trifluoroacetic acidHCID 14798Sodium HydroxideHCID 68958084HCID 68958084、化合物

生成物 1

HCID 576679632-(4-Fluoroanilino)-4-(isoquinolin-4-yl)benzoic acid収率 52.6%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

Trifluoroacetic acid 3.0 mL solution of tert-butyl 2-(4-fluoroanilino)-4-(isoquinolin-4-yl)benzoate 110 mg was stirred at room temperature for 1 hour. Water and ethyl acetate were added to the reaction mixture, and it was adjusted to pH6.0 with 1.0 mol/L sodium hydroxide aqueous solution. The organic layer was separated and collected,dried over anhydrous magnesium sulfate after washing with saturated sodium chloride aqueous solution, and the solvent was removed under reduced pressure. Hexane and diisopropyl ether were added to the obtained residue, and solid matter was filtrated to give 2-(4-fluoroanilino)-4-(isoquinolin-4-yl)benzoic acid 50 mg of pale green solid.

後処理

  1. customThe organic layer was separated
  2. washafter washing with saturated sodium chloride aqueous solution
  3. customthe solvent was removed under reduced pressure
  4. additionHexane and diisopropyl ether were added to the obtained residue, and solid matter
  5. filtrationwas filtrated

出典と根拠

ORDレコード
ord-5fe0d9119cd94ae4b3bbdd1bc051b248
出典データセット
uspto-grants-2012_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08327467B2

反応ノート

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