Sodium Bicarbonate → HCID 178474043, 화합물

HRID 392586노트

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HRID 392586 반응식
[OH:1][C:2]([C:30]1[CH:31]=[C:32]2[C:37](=[CH:38][CH:39]=1)[CH:36]=[C:35]([NH:40][C:41](=[O:43])[CH3:42])[CH:34]=[CH:33]2)([C:6]1[N:7]=[CH:8][N:9](C(C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[CH:10]=1)[CH:3]([CH3:5])[CH3:4].Cl.N1C=CC=CC=1.C(=O)([O-])O.[Na+]>CO>[OH:1][C:2]([C:30]1[CH:31]=[C:32]2[C:37](=[CH:38][CH:39]=1)[CH:36]=[C:35]([NH:40][C:41](=[O:43])[CH3:42])[CH:34]=[CH:33]2)([C:6]1[N:7]=[CH:8][NH:9][CH:10]=1)[CH:3]([CH3:5])[CH3:4]

참가 물질

5

반응물 3

HCID 516892Sodium BicarbonateHCID 10176127Pyridinium chlorideHCID 22018433HCID 22018433, 화합물

생성물 1

HCID 178474043HCID 178474043, 화합물수율 84%

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
60 °C

실험 절차

N-{6-[1-Hydroxy-2-methyl-1-(1-trityl-1H-imidazol-4-yl)propyl]naphthalen-2-yl}acetamide (11.5 g) and pyridine hydrochloride (390 mg) were dissolved in methanol (8 ml) and the mixture was stirred at 60° C. for 2 h. After allowing to cool, the mixture was neutralized with saturated aqueous sodium hydrogen carbonate. The solvent was evaporated and the residue was collected by filtration and washed with ethanol. The filtrate was concentrated and the obtained residue was purified by silica gel column chromatography (eluate, dichloromethane:methanol =30:1→10:1) and recrystallized from ethyl acetate to give the title compound (5.52 g) as a pale-red powder.

후처리

  1. temperatureto cool
  2. customThe solvent was evaporated
  3. filtrationthe residue was collected by filtration
  4. washwashed with ethanol
  5. concentrationThe filtrate was concentrated
  6. customthe obtained residue was purified by silica gel column chromatography (eluate, dichloromethane:methanol =30:1→10:1)
  7. customrecrystallized from ethyl acetate

출처 및 근거

ORD 기록
ord-1cd844a03f744ff7be025c69766b4d69
출처 데이터셋
uspto-grants-2004_10
특허 번호
US06800778B1

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