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Methyl iodide → 7-(3-(1-Methoxyethyl)Phenyl)-1-phenyl-5-trifluoromethylbenzimidazole

HRID 644536
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HRID 644536 반응식
[OH:1][CH:2]([C:4]1[CH:5]=[C:6]([C:10]2[C:15]3[N:16]([C:19]4[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=4)[CH:17]=[N:18][C:14]=3[CH:13]=[C:12]([C:25]([F:28])([F:27])[F:26])[CH:11]=2)[CH:7]=[CH:8][CH:9]=1)[CH3:3].[H-].[Na+].[H][H].I[CH3:34]>CN(C=O)C.O>[CH3:34][O:1][CH:2]([C:4]1[CH:5]=[C:6]([C:10]2[C:15]3[N:16]([C:19]4[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=4)[CH:17]=[N:18][C:14]=3[CH:13]=[C:12]([C:25]([F:28])([F:27])[F:26])[CH:11]=2)[CH:7]=[CH:8][CH:9]=1)[CH3:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 11372470HCID 11372470, 화합물HCID 178418361HCID 178418361, 화합물

생성물 1

HCID 113384407-(3-(1-Methoxyethyl)Phenyl)-1-phenyl-5-trifluoromethylbenzimidazole수율 37%

시약·촉매·용매 2

HCID 962Water
용매
HCID 6228Dimethylformamide용매

실험 절차

To a stirred solution of 7-(3-(1-hydroxyethyl)phenyl)-1-phenyl-5-trifluoromethylbenzimidazole (0.9 g, 2.4 mmol) in anhydrous DMF (5 ml) was added sodium hydride (0.15 g 60% dispersion in mineral oil, 3.5 mmol) at ambient temperature. When the evolution of hydrogen had ceased iodomethane (0.25 ml, 2.6 mmol) was added and stirring was continued for 15 min. Four volumes of water was added and the resultant mixture was extracted with ethyl acetate. This extract was washed twice with aqueous calcium chloride (3M), dried over magnesium sulphate and evaporated under reduced pressure. The residue was eluted through silica gel with a mixture of ethyl acetate and petroleum ether (2:3, v/v). Trituration of the concentrated eluate in ligroin afforded the title product (0.35 g, 37%) m/z, 397.2 (M+H)+.

후처리

  1. additionwas added
  2. extractionthe resultant mixture was extracted with ethyl acetate
  3. washThis extract was washed twice with aqueous calcium chloride (3M)
  4. dry with materialdried over magnesium sulphate
  5. customevaporated under reduced pressure
  6. washThe residue was eluted through silica gel with a mixture of ethyl acetate and petroleum ether (2:3

출처 및 근거

ORD 기록
ord-a758a711e4b74f5eb843d5e8610b26be
출처 데이터셋
uspto-grants-2010_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07700638B2

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