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Ammonium formate → 4-[4-(4-fluorophenyl)-1-hydroxy-1-(4-tert-butylaminocarbonylphenyl)butyl]-1H-imidazole

HRID 744724
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인쇄 미리보기

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HRID 744724 반응식
Cl.C([N:9]1[C:13]([C:14]([OH:38])([C:25]2[CH:30]=[CH:29][C:28]([C:31]([NH:33][C:34]([CH3:37])([CH3:36])[CH3:35])=[O:32])=[CH:27][CH:26]=2)[CH2:15][CH2:16][CH2:17][C:18]2[CH:23]=[CH:22][C:21]([F:24])=[CH:20][CH:19]=2)=[CH:12][N:11]=[CH:10]1)C1C=CC=CC=1.C([O-])=O.[NH4+]>[Pd].C(O)C>[F:24][C:21]1[CH:22]=[CH:23][C:18]([CH2:17][CH2:16][CH2:15][C:14]([C:13]2[N:9]=[CH:10][NH:11][CH:12]=2)([OH:38])[C:25]2[CH:30]=[CH:29][C:28]([C:31]([NH:33][C:34]([CH3:35])([CH3:36])[CH3:37])=[O:32])=[CH:27][CH:26]=2)=[CH:19][CH:20]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 2723923Ammonium formateHCID 194220141-benzyl-5-[4-(4-fluorophenyl)-1-hydroxy-1-(4-tert-butylaminocarbonylphenyl)butyl]-1H-imidazole hydrochloride

생성물 1

HCID 1784493104-[4-(4-fluorophenyl)-1-hydroxy-1-(4-tert-butylaminocarbonylphenyl)butyl]-1H-imidazole수율 79%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 702
Ethanol
용매

실험 절차

1-benzyl-5-[4-(4-fluorophenyl)-1-hydroxy-1-(4-tert-butylaminocarbonylphenyl)butyl]-1H-imidazole hydrochloride (12,95 g) is dissolved into aqueous ethanol (400 ml) and 1,3 g of 10% Pd/C is added. Ammonium formate (8,17 g) is added to the boiling solution in small portions. The mixture is refluxed for three hours. Then the reaction mixture is filtered through siliceous earth and the filtrate is evaporated to dryness. The residue is dissolved to methylene chloride, washed with 2M sodiumhydroxide and water, dried and evaporated to dryness. Yield 79%.

후처리

  1. additionis added
  2. temperatureThe mixture is refluxed for three hours
  3. filtrationThen the reaction mixture is filtered through siliceous earth
  4. customthe filtrate is evaporated to dryness
  5. dissolutionThe residue is dissolved to methylene chloride
  6. washwashed with 2M sodiumhydroxide and water
  7. customdried
  8. customevaporated to dryness

출처 및 근거

ORD 기록
ord-c16b678e3e844f2f9de1b75692c34f48
출처 데이터셋
uspto-grants-1996_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05559141

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