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Water → HCID 178446132, 화합물

HRID 730008
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HRID 730008 반응식
[C:1]([C:5]1[NH:9][C:8]([C:10]2[N:15]=[C:14]([NH:16][CH2:17][C:18]([CH3:21])([CH3:20])[CH3:19])[C:13]([N+:22]([O-])=O)=[CH:12][CH:11]=2)=[C:7]([C:25]2[CH:30]=[CH:29][C:28]([F:31])=[CH:27][CH:26]=2)[N:6]=1)([CH3:4])([CH3:3])[CH3:2].[N:32]#[C:33]Br.C(OCC)(=O)C.O>[Pd].C(O)C.CO.C(Cl)Cl>[NH3:6].[C:1]([C:5]1[NH:6][C:7]([C:25]2[CH:30]=[CH:29][C:28]([F:31])=[CH:27][CH:26]=2)=[C:8]([C:10]2[N:15]=[C:14]3[N:16]([CH2:17][C:18]([CH3:21])([CH3:20])[CH3:19])[C:33]([NH2:32])=[N:22][C:13]3=[CH:12][CH:11]=2)[N:9]=1)([CH3:4])([CH3:3])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

10

반응물 4

HCID 962WaterHCID 8857Ethyl AcetateHCID 10476Cyanogen BromideHCID 68867957HCID 68867957, 화합물

생성물 2

HCID 222AmmoniaHCID 178446132HCID 178446132, 화합물수율 74.2%

시약·촉매·용매 4

HCID 23938
Palladium
촉매
HCID 702Ethanol용매
HCID 887Methanol용매
HCID 6344Dichloromethane용매

실험 절차

Stir a suspension of {6-[2-tert-Butyl-5-(4-fluoro-phenyl)-3H-imidazol-4-yl]-3-nitro-pyridin-2-yl}-(2,2-dimethylpropyl)-amine (426 mg, 1.0 mmol) and 10% palladium on carbon (85 mg) in 100% ethanol under hydrogen from a balloon overnight. Filter the suspension through a 0.2 μm syringe filter and concentrate under reduced pressure. Dissolve the residue in 10% aqueous ethanol and treat at room temperature with cyanogen bromide (80 mg, 0.75 mmol, 1.5 equiv). When the reaction is complete, quench the reaction with saturated aqueous NaHCO3. Add ethyl acetate and water to dissolve all solids. Wash the organic layer once with saturated aqueous NaHCO3, once with saturated aqueous NaCl, dry with Na2SO4, filter, and concentrate under reduced pressure. Subject the residue to medium pressure silica gel chromatography eluting with 50% ethyl acetate/CH2Cl2 then with a gradient of 1.5-3.5% (2M ammonia in MeOH)/CH2Cl2) to provide 5-[2-tert-butyl-5-(4-fluoro-phenyl)-1H-imidazol-4-yl]-3-(2,2-dimethyl-propyl)-3H-imidazo[4,5-b]pyridin-2-ylamine as a brown foam (156 mg, 74% yield).

후처리

  1. filtrationFilter the suspension through a 0.2 μm syringe
  2. filtrationfilter
  3. concentrationconcentrate under reduced pressure
  4. dissolutionDissolve the residue in 10% aqueous ethanol
  5. customquench
  6. customthe reaction with saturated aqueous NaHCO3
  7. washWash the organic layer once with saturated aqueous NaHCO3
  8. dry with materialonce with saturated aqueous NaCl, dry with Na2SO4
  9. filtrationfilter
  10. concentrationconcentrate under reduced pressure
  11. washeluting with 50% ethyl acetate/CH2Cl2

출처 및 근거

ORD 기록
ord-c2fe895bf56e4317a1c991fd8b31d2be
출처 데이터셋
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07582652B2

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