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Imidazole → HCID 22504276, 화합물

HRID 651431
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HRID 651431 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([CH2:8]Cl)[CH:5]=[C:4]([Cl:10])[N:3]=1.[Si:11](Cl)([C:14]([CH3:17])([CH3:16])[CH3:15])([CH3:13])[CH3:12].CN(C)C=[O:22].N1C=CN=C1>C(OCC)(=O)C>[Cl:1][C:2]1[CH:7]=[C:6]([CH2:8][O:22][Si:11]([C:14]([CH3:17])([CH3:16])[CH3:15])([CH3:13])[CH3:12])[CH:5]=[C:4]([Cl:10])[N:3]=1
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참가 물질

6

반응물 4

HCID 795ImidazoleHCID 6228DimethylformamideHCID 28928tert-Butyldimethylsilyl chlorideHCID 27946262,6-dichloro-4-(chloromethyl)pyridine

생성물 1

HCID 22504276HCID 22504276, 화합물

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

0.30 g of 2,6-dichloro-4-chloromethylpyridine and 0.25 g of tert-butyldimethylsilyl chloride were added to 4.0 ml of dimethylformamide, and were dissolved. The solution was cooled in an ice bath. After 0.14 g of imidazole was added, stirring was conducted at room temperature for 5.5 hours. Ethyl acetate was added to the reacted solution. The organic phase was washed with water, and was dried by adding sodium sulfate. The solvent was removed by evaporation, and the residue was purified by silica gel column chromatography to obtain 0.41 g of 2,6-dichloro-4-((1,1-dimethylethyl)dimethylsilyl)oxymethylpyridine (Compound No. 96).

후처리

  1. dissolutionwere dissolved
  2. temperatureThe solution was cooled in an ice bath
  3. washThe organic phase was washed with water
  4. customwas dried
  5. additionby adding sodium sulfate
  6. customThe solvent was removed by evaporation
  7. customthe residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-32287cc5a2b14dcdaca6751c9fdf6dc3
출처 데이터셋
uspto-grants-2001_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06281231B1

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