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

HRID 2266742

반응식

HRID 2266742 반응식
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]

참가 물질

5

반응물 2

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

생성물 1

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

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

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

후처리

  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

출처 및 근거

ORD 기록
ord-1f278d4a0d234f839d9ded73a6540a0a
출처 데이터셋
uspto-grants-2010_12
특허 번호
US07858654B2

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