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Imidazole → tert-Butyldimethyl(4-nitrophenoxy)silane

HRID 7236
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HRID 7236 반응식
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([OH:10])=[CH:6][CH:5]=1)([O-:3])=[O:2].N1C=CN=C1.[Si:16](Cl)([C:19]([CH3:22])([CH3:21])[CH3:20])([CH3:18])[CH3:17]>CN(C)C=O>[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([O:10][Si:16]([CH3:18])([CH3:17])[C:19]([CH3:22])([CH3:21])[CH3:20])=[CH:6][CH:5]=1)([O-:3])=[O:2]
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참가 물질

5

반응물 3

HCID 795ImidazoleHCID 9804-NitrophenolHCID 28928tert-Butyldimethylsilyl chloride2회

생성물 1

HCID 532659tert-Butyldimethyl(4-nitrophenoxy)silane

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution of 4-nitrophenol (5.0 g, 35.9 mmol) (Aldrich) in dimethylformamide (50 mL) was added imidazole (3.18 g, 46.7 mmol) (Aldrich) and t-butyldimethylsilyl chloride (6.49 g, 43.1 mmol) (Avocado Research Chemicals Ltd.). The reaction mixture was stirred at room temperature for 1 day. TLC analysis showed starting material was still present. Another portion of t-butyldimethylsilyl chloride (1.0 g, 6.63 mmol) was added and the mixture was stirred at room temperature for another 1 day. The reaction mixture was concentrated under reduced pressure. The residue was dissolved in ethyl acetate (200 mL) and washed with a mixture of water (100 mL) and aqueous 1N HCl (80 mL). The organic layer was then washed with water, saturated aqueous sodium bicarbonate solution and brine, dried (MgSO4), filtered and concentrated. The residue was purified by flash chromatography eluting with ethyl acetate/hexanes (1:9, V/V) to afford 1-nitro-4-(1,1,2,2-tetramethyl-1-silapropoxy)benzene. (Yield 7.8 g, 86%).

후처리

  1. stirringthe mixture was stirred at room temperature for another 1 day
  2. concentrationThe reaction mixture was concentrated under reduced pressure
  3. dissolutionThe residue was dissolved in ethyl acetate (200 mL)
  4. washwashed with a mixture of water (100 mL) and aqueous 1N HCl (80 mL)
  5. washThe organic layer was then washed with water, saturated aqueous sodium bicarbonate solution and brine
  6. dry with materialdried (MgSO4)
  7. filtrationfiltered
  8. concentrationconcentrated
  9. customThe residue was purified by flash chromatography
  10. washeluting with ethyl acetate/hexanes (1:9, V/V)

출처 및 근거

ORD 기록
ord-fdb8a9152bfd4faca050f70d5c0c0d5b
출처 데이터셋
uspto-grants-2006_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07084270B2

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