Imidazole → HCID 13007323, 화합물

HRID 990606노트

반응식

HRID 990606 반응식
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]

참가 물질

6

반응물 4

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

생성물 1

HCID 13007323HCID 13007323, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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:

후처리

  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

출처 및 근거

ORD 기록
ord-4729ed42625648a6a0ca9f5092872787
출처 데이터셋
uspto-grants-2002_10
특허 번호
US06461876B1

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