Imidazole → HCID 13007323、化合物

HRID 2220029ノート

反応式

HRID 2220029 の反応式
CN(C)C=O.[OH:6][C:7]1[CH:8]=[C:9]([CH:18]=[CH:19][CH:20]=1)[C:10]([O:12][CH2:13][C:14]([F:17])([F:16])[F:15])=[O:11].[C:21]([Si:25](Cl)([CH3:27])[CH3:26])([CH3:24])([CH3:23])[CH3:22].N1C=CN=C1>O>[O:6]([C:7]1[CH:8]=[C:9]([CH:18]=[CH:19][CH:20]=1)[C:10]([O:12][CH2:13][C:14]([F:15])([F:16])[F:17])=[O:11])[Si:25]([C:21]([CH3:24])([CH3:23])[CH3:22])([CH3:27])[CH3:26]

参加物

6

反応物 4

HCID 795ImidazoleHCID 6228DimethylformamideHCID 28928tert-Butyldimethylsilyl chlorideHCID 130073222,2,2-Trifluoroethyl 3-hydroxybenzoate

生成物 1

HCID 13007323HCID 13007323、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Into a 250 mL round bottom flask was added 30 mL of dry dimethyl formamide and 4.0 parts of ester (47) and 3.5 parts of tert-butyldimethyl silyl chloride were added to the reaction flask with stirring. Three parts of Imidazole was added in portions and stirring was continued for 10 hours. The reaction mixture was diluted with 80 mL of water and the product was extracted with ethyl acetate. The organic layer was washed with water and dried on anhydrous sodium sulfate. The solvent was evaporated under reduced pressure to give an oil, yield 5.65 parts. The structure was confirmed on the basis of 1H NMR. The reaction proceeded as follows:

後処理

  1. additionwere added to the reaction flask
  2. stirringstirring
  3. extractionthe product was extracted with ethyl acetate
  4. washThe organic layer was washed with water
  5. dry with materialdried on anhydrous sodium sulfate
  6. customThe solvent was evaporated under reduced pressure
  7. customto give an oil
  8. customyield 5.65 parts

出典と根拠

ORDレコード
ord-32ae9a2f1a4d499ba596f12f8337a427
出典データセット
uspto-grants-2008_08
特許番号
US07416898B2

反応ノート

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