Lithium hydroxide, monohydrate → 5-(2-Ethyl-imidazol-1-yl)-4'-methyl-biphenyl-3-carboxylic acid

HRID 2266742

反応式

HRID 2266742 の反応式
C[O:2][C:3]([C:5]1[CH:6]=[C:7]([C:18]2[CH:23]=[CH:22][C:21]([CH3:24])=[CH:20][CH:19]=2)[CH:8]=[C:9]([N:11]2[CH:15]=[CH:14][N:13]=[C:12]2[CH2:16][CH3:17])[CH:10]=1)=[O:4].O[Li].O>C1COCC1.O>[CH2:16]([C:12]1[N:11]([C:9]2[CH:10]=[C:5]([C:3]([OH:4])=[O:2])[CH:6]=[C:7]([C:18]3[CH:23]=[CH:22][C:21]([CH3:24])=[CH:20][CH:19]=3)[CH:8]=2)[CH:15]=[CH:14][N:13]=1)[CH3:17]

参加物

5

反応物 2

HCID 168937Lithium hydroxide, monohydrateHCID 577497845-(2-Ethyl-imidazol-1-yl)-4'-methyl-biphenyl-3-carboxylic acid methyl ester

生成物 1

HCID 577497835-(2-Ethyl-imidazol-1-yl)-4'-methyl-biphenyl-3-carboxylic acid

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

5-(2-Ethyl-imidazol-1-yl)-4′-methyl-biphenyl-3-carboxylic acid methyl ester (750 mg) was dissolved in THF (14 mL) and water (8 mL), and LiOH hydrate (128 mg, 3.1 mmol) was added as one portion. The reaction mixture was stirred at room temperature for 3 hours, then THF was removed under reduced pressure. Concentrated HCl was added into the remaining aqueous solution to adjust the pH to ˜6. The solution was extracted with EtOAc, and the combined organic layers were dried over anhydrous sodium sulfate, filtered, and concentrated under reduced pressure to give 5-(2-ethyl-imidazol-1-yl)-4′-methyl-biphenyl-3-carboxylic acid

後処理

  1. customTHF was removed under reduced pressure
  2. additionConcentrated HCl was added into the remaining aqueous solution
  3. extractionThe solution was extracted with EtOAc
  4. dry with materialthe combined organic layers were dried over anhydrous sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-1f278d4a0d234f839d9ded73a6540a0a
出典データセット
uspto-grants-2010_12
特許番号
US07858654B2

関連ノート

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