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Imidazole → HCID 22504276、化合物

HRID 651431
ノート
印刷プレビュー

反応式

HRID 651431 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

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

生成物 1

HCID 22504276HCID 22504276、化合物

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-32287cc5a2b14dcdaca6751c9fdf6dc3
出典データセット
uspto-grants-2001_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06281231B1

反応ノート

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