Trifluoroacetic acid → 4-Phenyl-2-(4-phenylpyridine-2-carboxamido)benzoic acid

HRID 454776ノート

反応式

HRID 454776 の反応式
FC(F)(F)C(O)=O.[C:8]1([C:14]2[CH:26]=[CH:25][C:17]([C:18]([O:20]C(C)(C)C)=[O:19])=[C:16]([NH:27][C:28]([C:30]3[CH:35]=[C:34]([C:36]4[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=4)[CH:33]=[CH:32][N:31]=3)=[O:29])[CH:15]=2)[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1>>[C:8]1([C:14]2[CH:26]=[CH:25][C:17]([C:18]([OH:20])=[O:19])=[C:16]([NH:27][C:28]([C:30]3[CH:35]=[C:34]([C:36]4[CH:37]=[CH:38][CH:39]=[CH:40][CH:41]=4)[CH:33]=[CH:32][N:31]=3)=[O:29])[CH:15]=2)[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1

参加物

3

反応物 2

HCID 6422Trifluoroacetic acidHCID 58508724Tert-butyl 4-phenyl-2-(4-phenylpyridine-2-carboxamido)benzoate

生成物 1

HCID 585089074-Phenyl-2-(4-phenylpyridine-2-carboxamido)benzoic acid収率 89.2%

実験手順

Trifluoroacetic acid (5 mL) was added to the obtained tert-butyl 4-phenyl-2-(4-phenylpyridine-2-carboxamido)benzoate (64 mg), followed by stirring at room temperature for 3 hours. The solvent was evaporated under reduced pressure, and ethyl acetate and water were added to the obtained residue. After adjusting the pH to 6.5 with a saturated aqueous solution of sodium bicarbonate, the organic layer was separated, washed with water and a saturated aqueous solution of sodium chloride sequentially, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. Diisopropyl ether was added to the obtained residue, and the solid substance was collected by filtration to obtain 50 mg of 4-phenyl-2-(4-phenylpyridine-2-carboxamido)benzoic acid as a white solid.

後処理

  1. customThe solvent was evaporated under reduced pressure, and ethyl acetate and water
  2. additionwere added to the obtained residue
  3. customthe organic layer was separated
  4. washwashed with water
  5. dry with materiala saturated aqueous solution of sodium chloride sequentially, and dried over anhydrous magnesium sulfate
  6. customthe solvent was evaporated under reduced pressure
  7. additionDiisopropyl ether was added to the obtained residue
  8. filtrationthe solid substance was collected by filtration

出典と根拠

ORDレコード
ord-a68ca11a4c074c5b8bc80ff71709218a
出典データセット
uspto-grants-2013_07
特許番号
US08492582B2

反応ノート

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