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Sodium Bicarbonate → HCID 178450128, 화합물

HRID 1059144
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HRID 1059144 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:13]=[CH:12][CH:11]=[C:10]([C:14]([C:19]3[N:20]=[CH:21][N:22](C(C4C=CC=CC=4)(C4C=CC=CC=4)C4C=CC=CC=4)[CH:23]=3)([OH:18])[CH:15]([CH3:17])[CH3:16])[CH:9]=2)=[CH:4][CH:3]=1.Cl.N1C=CC=CC=1.C(=O)([O-])O.[Na+]>CO>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:13]=[CH:12][CH:11]=[C:10]([C:14]([C:19]3[N:20]=[CH:21][NH:22][CH:23]=3)([OH:18])[CH:15]([CH3:17])[CH3:16])[CH:9]=2)=[CH:4][CH:3]=1
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참가 물질

5

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HCID 516892Sodium BicarbonateHCID 10176127Pyridinium chlorideHCID 186685501-(4'-chloro[1,1'-biphenyl]-3-yl)-2-methyl-1-(1-trityl-1H-imidazol-4-yl)-1-propanol

생성물 1

HCID 178450128HCID 178450128, 화합물수율 76%

시약·촉매·용매 1

HCID 887Methanol용매

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온도
60 °C

실험 절차

1-(4′-Chloro[1,1′-biphenyl]-3-yl)-2-methyl-1-(1-trityl-1H-imidazol-4-yl)-1-propanol (0.71 g) and pyridine hydrochloride (0.25 g) were dissolved in methanol (20 ml), and the mixture was stirred at 60° C. for 2 h. To the reaction mixture was added saturated aqueous sodium hydrogen carbonate solution and the mixture was concentrated. Water and ethyl acetate were added and the mixture was extracted with ethyl acetate. The organic layer was dried and concentrated, and the obtained residue was purified by silica gel column chomatography (eluent, dichloromethane:methanol=40:1). Recrystallization from hexane-ethyl acetate gave the title compound (0.31 g) as a colorless solid.

후처리

  1. concentrationthe mixture was concentrated
  2. additionWater and ethyl acetate were added
  3. extractionthe mixture was extracted with ethyl acetate
  4. customThe organic layer was dried
  5. concentrationconcentrated
  6. customthe obtained residue was purified by silica gel column chomatography (eluent, dichloromethane:methanol=40:1)
  7. customRecrystallization from hexane-ethyl acetate

출처 및 근거

ORD 기록
ord-a9692b3c177c41cc92753d35db0f7782
출처 데이터셋
uspto-grants-2003_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06518257B1

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