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1-(1H-Imidazol-4-yl)-1-(naphtho[2,1-b]furan-7-yl)-2-methyl-1-propanol → HCID 178450034, 화합물

HRID 480468
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HRID 480468 반응식
[NH:1]1[CH:5]=[C:4]([C:6]([C:11]2[CH:12]=[C:13]3[C:21](=[CH:22][CH:23]=2)[C:20]2[CH:19]=[CH:18][O:17][C:16]=2[CH:15]=[CH:14]3)([OH:10])[CH:7]([CH3:9])[CH3:8])[N:3]=[CH:2]1>C(O)(=O)C.[C].[Rh]>[CH2:19]1[CH2:18][O:17][C:16]2[CH:15]=[CH:14][C:13]3[C:21]([C:20]1=2)=[CH:22][CH:23]=[C:11]([C:6]([C:4]1[N:3]=[CH:2][NH:1][CH:5]=1)([OH:10])[CH:7]([CH3:9])[CH3:8])[CH:12]=3
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참가 물질

4

반응물 1

HCID 1784500551-(1H-Imidazol-4-yl)-1-(naphtho[2,1-b]furan-7-yl)-2-methyl-1-propanol

생성물 1

HCID 178450034HCID 178450034, 화합물수율 34.3%

시약·촉매·용매 2

HCID 178503043HCID 178503043, 화합물촉매HCID 176Acetic Acid용매

실험 절차

A mixture of 1-(1H-imidazol-4-yl)-1-(naphtho[2,1-b]furan-7-yl)-2-methyl-1-propanol (0.310 g) and 5% rhodium carbon (1.50 g) in acetic acid (50 mL) was stirred at room temperature for 7 h under hydrogen atmosphere at 4 atom pressure. Catalyst was filtered off, and the filtrate was concentrated. The residue was dissolved in ethyl acetate, washed with saturated sodium bicarbonate solution and brine, dried and concentrated. The residue was chromatographed on silica gel (eluent; dichloromethane:methanol=20:1) followed by crystallization from ethyl acetate to give the titled compound (0.107 g) as a colorless solid.

후처리

  1. filtrationCatalyst was filtered off
  2. concentrationthe filtrate was concentrated
  3. dissolutionThe residue was dissolved in ethyl acetate
  4. washwashed with saturated sodium bicarbonate solution and brine
  5. customdried
  6. concentrationconcentrated
  7. customThe residue was chromatographed on silica gel (eluent; dichloromethane:methanol=20:1)
  8. customfollowed by crystallization from ethyl acetate

출처 및 근거

ORD 기록
ord-ccebd620045d4243b0d1f0c44a67cd15
출처 데이터셋
uspto-grants-2003_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06649643B1

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