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Trifluoroacetic acid → 4-(2-Fluorophenyl)-2-(5-phenylpyridine-3-carboxamido)benzoic acid

HRID 454759
ノート
印刷プレビュー

反応式

HRID 454759 の反応式
FC(F)(F)C(O)=O.[F:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=1[C:15]1[CH:27]=[CH:26][C:18]([C:19]([O:21]C(C)(C)C)=[O:20])=[C:17]([NH:28][C:29]([C:31]2[CH:32]=[N:33][CH:34]=[C:35]([C:37]3[CH:42]=[CH:41][CH:40]=[CH:39][CH:38]=3)[CH:36]=2)=[O:30])[CH:16]=1>>[F:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=1[C:15]1[CH:27]=[CH:26][C:18]([C:19]([OH:21])=[O:20])=[C:17]([NH:28][C:29]([C:31]2[CH:32]=[N:33][CH:34]=[C:35]([C:37]3[CH:42]=[CH:41][CH:40]=[CH:39][CH:38]=3)[CH:36]=2)=[O:30])[CH:16]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 2

HCID 6422Trifluoroacetic acidHCID 58508706Tert-butyl 4-(2-fluorophenyl)-2-(5-phenylpyridine-3-carboxamido)benzoate

生成物 1

HCID 585085154-(2-Fluorophenyl)-2-(5-phenylpyridine-3-carboxamido)benzoic acid

実験手順

Trifluoroacetic acid (3.0 mL) was added to the obtained tert-butyl 4-(2-fluorophenyl)-2-(5-phenylpyridine-3-carboxamido)benzoate, followed by stirring at room temperature for 1 hour and 30 minutes. The solvent was evaporated under reduced pressure, and diisopropyl ether was added to the obtained residue. The solid substance was collected by filtration. Dioxane (3.0 mL) and a 2 mol/L aqueous solution of sodium hydroxide (0.041 mL) were added to the obtained solid substance, followed by stirring at room temperature for 1 hour. A 10% aqueous solution of citric acid was added to the reaction mixture, and the solid substance was collected by filtration to obtain 36 mg of 4-(2-fluorophenyl)-2-(5-phenylpyridine-3-carboxamido)benzoic acid as a white solid.

後処理

  1. customThe solvent was evaporated under reduced pressure, and diisopropyl ether
  2. additionwas added to the obtained residue
  3. filtrationThe solid substance was collected by filtration
  4. additionDioxane (3.0 mL) and a 2 mol/L aqueous solution of sodium hydroxide (0.041 mL) were added to the obtained solid substance
  5. stirringby stirring at room temperature for 1 hour
  6. additionA 10% aqueous solution of citric acid was added to the reaction mixture
  7. filtrationthe solid substance was collected by filtration

出典と根拠

ORDレコード
ord-fd64c3afc8fa4d918ef78f2dde168b2e
出典データセット
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08492582B2

反応ノート

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