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Imidazole → HCID 23017932, 화합물

HRID 1616724
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HRID 1616724 반응식
N1C=CN=C1.[CH3:6][S:7]([C:10]1[CH:15]=[CH:14][C:13]([OH:16])=[CH:12][CH:11]=1)(=[O:9])=[O:8].[C:17]([Si:21]([CH3:24])([CH3:23])Cl)([CH3:20])([CH3:19])[CH3:18]>CN(C)C=O.[Cl-].[Na+].O>[C:17]([Si:21]([O:16][C:13]1[CH:14]=[CH:15][C:10]([S:7]([CH3:6])(=[O:8])=[O:9])=[CH:11][CH:12]=1)([CH3:24])[CH3:23])([CH3:20])([CH3:19])[CH3:18]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 795ImidazoleHCID 28928tert-Butyldimethylsilyl chlorideHCID 1233504-(Methylsulfonyl)phenol

생성물 1

HCID 23017932HCID 23017932, 화합물수율 96%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 57417360Sodium chloride; water용매

실험 절차

9.9 g (145.18 mmol) of imidazole was added to and dissolved in an N,N-dimethylformamide solution (150 mL) of 10 g (58.07 mmol) of 4-methylsulfonylphenol, and then 10.5 g (69.7 mmol) of tert-butyldimethylchlorosilane was added thereto and stirred. After the reaction, brine was added thereto and extracted with ethyl acetate. The organic layer was washed three times with brine, and dried over anhydrous magnesium sulfate. Purifying by silica gel column chromatography (hexane/ethyl acetate=5/1→3/1) gave 15.97 g (55.75 mmol) of tert-butyl-(4-methanesulfonylphenoxy)dimethylsilane (XII-6) (yield 96%). Its physical properties are shown below.

후처리

  1. additionwas added
  2. extractionextracted with ethyl acetate
  3. washThe organic layer was washed three times with brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customPurifying by silica gel column chromatography (hexane/ethyl acetate=5/1→3/1)

출처 및 근거

ORD 기록
ord-d981c0048d6c4022bcb249a50669402d
출처 데이터셋
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08765814B2

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