1,4-Dioxane → 2-(2-Fluoro-5-nitrophenyl)pyridine

HRID 13286

반응식

HRID 13286 반응식
Br[C:2]1[CH:3]=[C:4]([N+:9]([O-:11])=[O:10])[CH:5]=[CH:6][C:7]=1[F:8].C(=O)(O)[O-].[Na+].O1[CH2:22][CH2:21]OCC1>>[F:8][C:7]1[CH:6]=[CH:5][C:4]([N+:9]([O-:11])=[O:10])=[CH:3][C:2]=1[C:22]1[CH:21]=[CH:2][CH:3]=[CH:4][N:9]=1

참가 물질

4

반응물 3

HCID 312751,4-DioxaneHCID 696992-Bromo-1-fluoro-4-nitrobenzeneHCID 516892Sodium Bicarbonate

생성물 1

HCID 222853002-(2-Fluoro-5-nitrophenyl)pyridine

실험 절차

0.55 g of Tetrakis-triphenylphosphine palladium was added to a 1,4-dioxane (20 ml) solution of 2.1 g of 3-bromo-4-fluoro-nitrobenzene and 2.3 g of 2-trimethyltin-pyridine, and the reaction liquid was heated overnight under reflux. Aqueous saturated sodium bicarbonate was added to the reaction liquid, and extracted with ethyl acetate. The organic layer was washed with water and saturated saline, and dried with anhydrous sodium sulfate. The solvent was evaporated away under reduced pressure, and the resulting residue was purified through silica gel column chromatography (developing solvent: hexane/ethyl acetate=7/1) to obtain the entitled compound as a yellow solid.

후처리

  1. customthe reaction liquid
  2. temperaturewas heated overnight
  3. temperatureunder reflux
  4. extractionextracted with ethyl acetate
  5. washThe organic layer was washed with water and saturated saline
  6. dry with materialdried with anhydrous sodium sulfate
  7. customThe solvent was evaporated away under reduced pressure
  8. customthe resulting residue was purified through silica gel column chromatography (developing solvent: hexane/ethyl acetate=7/1)

출처 및 근거

ORD 기록
ord-b06ca7ffde7348cc9499a39a52f86f8f
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07728025B2

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