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Imidazole → HCID 57792032, 화합물

HRID 421988
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HRID 421988 반응식
[Br:1][C:2]1[CH:7]=[C:6]([N:8]([CH2:14][O:15][CH3:16])[C:9]2[S:10][CH:11]=[CH:12][N:13]=2)[N:5]=[C:4]([CH2:17][OH:18])[CH:3]=1.N1C=CN=C1.[Si:24](Cl)([C:27]([CH3:30])([CH3:29])[CH3:28])([CH3:26])[CH3:25]>CN(C)C=O.C(OCC)(=O)C>[Br:1][C:2]1[CH:3]=[C:4]([CH2:17][O:18][Si:24]([C:27]([CH3:30])([CH3:29])[CH3:28])([CH3:26])[CH3:25])[N:5]=[C:6]([N:8]([CH2:14][O:15][CH3:16])[C:9]2[S:10][CH:11]=[CH:12][N:13]=2)[CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 795ImidazoleHCID 28928tert-Butyldimethylsilyl chlorideHCID 57792034HCID 57792034, 화합물

생성물 1

HCID 57792032HCID 57792032, 화합물

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

18.5 g of (4-bromo-6-((methoxymethyl)(1,3-thiazol-2-yl)amino)pyridin-2-yl)-methanol was dissolved in 110 mL of dimethylformamide and 9.64 g of imidazole was added thereto. Under cooling with an ice bath, 10.2 g of tert-butyldimethylsilyl chloride was added thereto followed by stirring at room temperature for 3 hours. The reaction solution was diluted with ethyl acetate and washed with water and brine. The resulting organic layer was dried over magnesium sulfate and filtered, and the filtrate was concentrated. The resulting residue was purified by a silica gel column chromatography (eluent: hexane/ethyl acetate=9/1 to 4/1) to give the title compound.

후처리

  1. temperatureUnder cooling with an ice bath
  2. washwashed with water and brine
  3. dry with materialThe resulting organic layer was dried over magnesium sulfate
  4. filtrationfiltered
  5. concentrationthe filtrate was concentrated
  6. customThe resulting residue was purified by a silica gel column chromatography (eluent: hexane/ethyl acetate=9/1 to 4/1)

출처 및 근거

ORD 기록
ord-74fe00d96fc641729efd33f70ea595f7
출처 데이터셋
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08101621B2

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