Trifluoroacetic acid → 2-(2-Hydroxy-5-(methyl(2-(morpholin-4-yl)ethyl)amino)benzamido)-4-phenylbenzoic acid

HRID 454612ノート

反応式

HRID 454612 の反応式
FC(F)(F)C(O)=O.[OH:8][C:9]1[CH:36]=[CH:35][C:34]([N:37]([CH3:46])[CH2:38][CH2:39][N:40]2[CH2:45][CH2:44][O:43][CH2:42][CH2:41]2)=[CH:33][C:10]=1[C:11]([NH:13][C:14]1[CH:26]=[C:25]([C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=2)[CH:24]=[CH:23][C:15]=1[C:16]([O:18]C(C)(C)C)=[O:17])=[O:12]>>[OH:8][C:9]1[CH:36]=[CH:35][C:34]([N:37]([CH3:46])[CH2:38][CH2:39][N:40]2[CH2:45][CH2:44][O:43][CH2:42][CH2:41]2)=[CH:33][C:10]=1[C:11]([NH:13][C:14]1[CH:26]=[C:25]([C:27]2[CH:28]=[CH:29][CH:30]=[CH:31][CH:32]=2)[CH:24]=[CH:23][C:15]=1[C:16]([OH:18])=[O:17])=[O:12]

参加物

3

反応物 2

HCID 6422Trifluoroacetic acidHCID 58508749Tert-butyl 2-(2-hydroxy-5-(methyl(2-(morpholin-4-yl)ethyl)amino)benzamido)-4-phenylbenzoate

生成物 1

HCID 585089032-(2-Hydroxy-5-(methyl(2-(morpholin-4-yl)ethyl)amino)benzamido)-4-phenylbenzoic acid収率 36.3%

実験手順

Trifluoroacetic acid (5.0 mL) was added to the obtained tert-butyl 2-(2-hydroxy-5-(methyl(2-(morpholin-4-yl)ethyl)amino)benzamido)-4-phenylbenzoate (0.074 g), followed by stirring at room temperature for 3 hours. The solvent was evaporated under reduced pressure, and water and chloroform were added to the residue. After adjusting the pH to 7.0 with a saturated aqueous solution of sodium bicarbonate, the organic layer was separated, and the aqueous layer was extracted with chloroform. The organic layer and the extract were combined, and the resulting mixture was dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure, and diisopropyl ether was added to the obtained residue. The solid substance was collected by filtration to obtain 0.024 g of 2-(2-hydroxy-5-(methyl(2-(morpholin-4-yl)ethyl)amino)benzamido)-4-phenylbenzoic acid as a yellow solid.

後処理

  1. customThe solvent was evaporated under reduced pressure, and water and chloroform
  2. additionwere added to the residue
  3. customthe organic layer was separated
  4. extractionthe aqueous layer was extracted with chloroform
  5. dry with materialthe resulting mixture was dried over anhydrous sodium sulfate
  6. customThe solvent was evaporated under reduced pressure, and diisopropyl ether
  7. additionwas added to the obtained residue
  8. filtrationThe solid substance was collected by filtration

出典と根拠

ORDレコード
ord-8b772fa0d329438b9b9dd1a47bf4da2a
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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