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

HRID 454754ノート

反応式

HRID 454754 の反応式
FC(F)(F)C(O)=O.[CH3:8][O:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1[C:16]1[CH:28]=[CH:27][C:19]([C:20]([O:22]C(C)(C)C)=[O:21])=[C:18]([NH:29][C:30]([C:32]2[CH:33]=[N:34][CH:35]=[C:36]([C:38]3[CH:43]=[CH:42][CH:41]=[CH:40][CH:39]=3)[CH:37]=2)=[O:31])[CH:17]=1>>[CH3:8][O:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1[C:16]1[CH:28]=[CH:27][C:19]([C:20]([OH:22])=[O:21])=[C:18]([NH:29][C:30]([C:32]2[CH:33]=[N:34][CH:35]=[C:36]([C:38]3[CH:43]=[CH:42][CH:41]=[CH:40][CH:39]=3)[CH:37]=2)=[O:31])[CH:17]=1

参加物

3

実験手順

Trifluoroacetic acid (4.0 mL) was added to the obtained tert-butyl 4-(2-methoxyphenyl)-2-(5-phenylpyridine-3-carboxamido)benzoate (61 mg), followed by stirring at room temperature for 1 hour. The solvent was evaporated under reduced pressure, and diisopropyl ether was added to the obtained residue. The solid substance was collected by filtration, and dioxane (3.0 mL), water, and a 2 mol/L aqueous solution of sodium hydroxide (0.080 mL) were added to the obtained residue. After adjusting the pH to 7.6 with 1 mol/L hydrochloric acid, the solid substance was collected by filtration to obtain 32 mg of 4-(2-methoxyphenyl)-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, and dioxane (3.0 mL), water
  4. additiona 2 mol/L aqueous solution of sodium hydroxide (0.080 mL) were added to the obtained residue
  5. filtrationthe solid substance was collected by filtration

出典と根拠

ORDレコード
ord-01c3ae02dccf4815bbb5c39fa1aa2e0d
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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