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Trityl chloride → (2-Butyl-4-chloro-1-((2'-(1-trityl-1H-tetraazol-5-YL)(1,1'-biphenyl)-4-YL)methyl)-1H-imidazol-5-YL)methanol

HRID 487909
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HRID 487909 반응식
[K].[CH2:2]([C:6]1[N:7]([CH2:14][C:15]2[CH:20]=[CH:19][C:18]([C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=3[C:27]3[NH:31][N:30]=[N:29][N:28]=3)=[CH:17][CH:16]=2)[C:8]([CH2:12][OH:13])=[C:9]([Cl:11])[N:10]=1)[CH2:3][CH2:4][CH3:5].C(N(CC)CC)C.[C:39](Cl)([C:52]1[CH:57]=[CH:56][CH:55]=[CH:54][CH:53]=1)([C:46]1[CH:51]=[CH:50][CH:49]=[CH:48][CH:47]=1)[C:40]1[CH:45]=[CH:44][CH:43]=[CH:42][CH:41]=1>C(Cl)Cl.O>[CH2:2]([C:6]1[N:7]([CH2:14][C:15]2[CH:20]=[CH:19][C:18]([C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=3[C:27]3[N:31]([C:39]([C:40]4[CH:45]=[CH:44][CH:43]=[CH:42][CH:41]=4)([C:52]4[CH:53]=[CH:54][CH:55]=[CH:56][CH:57]=4)[C:46]4[CH:47]=[CH:48][CH:49]=[CH:50][CH:51]=4)[N:30]=[N:29][N:28]=3)=[CH:17][CH:16]=2)[C:8]([CH2:12][OH:13])=[C:9]([Cl:11])[N:10]=1)[CH2:3][CH2:4][CH3:5]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 6456Trityl chlorideHCID 8471TriethylamineHCID 98471641H-Imidazole-5-methanol, 2-butyl-4-chloro-1-[[2'-(2H-tetrazol-5-yl)[1,1'-biphenyl]-4-yl]methyl]-, potassium salt (1:1)

생성물 1

HCID 11643218(2-Butyl-4-chloro-1-((2'-(1-trityl-1H-tetraazol-5-YL)(1,1'-biphenyl)-4-YL)methyl)-1H-imidazol-5-YL)methanol수율 90.9%

시약·촉매·용매 2

HCID 962
Water
용매
HCID 6344Dichloromethane용매

실험 절차

To a solution of 0.600 g of 2-butyl-4-chloro-1-[[2'-(1H-tetrazol-5-yl)[1,1'-biphenyl]-4-yl]methyl]-1H-imidazole-5-methanol mono potassium salt in 40 ml of methylene chloride is added 0.218 ml of triethylamine and 0.381 g of trityl chloride. The solution is heated at reflux for 8 hours, cooled and diluted with 30 ml of water. The organic layer is separated and the aqueous layer extracted with methylene chloride. The combined extracts are washed with water, dried with potassium carbonate, filtered and concentrated in vacuo to give 0.785 g of the desired product as a solid. FAB MASS SPEC 665(M+H).

후처리

  1. temperatureThe solution is heated
  2. temperatureat reflux for 8 hours
  3. temperaturecooled
  4. customThe organic layer is separated
  5. extractionthe aqueous layer extracted with methylene chloride
  6. washThe combined extracts are washed with water
  7. dry with materialdried with potassium carbonate
  8. filtrationfiltered
  9. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-0b5002cf935344c28cdb4dcb039acb16
출처 데이터셋
uspto-grants-1994_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05298517

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