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Potassium Fluoride → 1-(5,6,7,8-Tetrahydroimidazo[1,2-a]pyridin-3-yl)ethanone

HRID 2238644
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HRID 2238644 반응식
Br[C:2]1[N:6]2[CH2:7][CH2:8][CH2:9][CH2:10][C:5]2=[N:4][CH:3]=1.C([Sn](CCCC)(CCCC)[C:16]([O:18]CC)=[CH2:17])CCC.[F-].[K+]>C1(C)C=CC=CC=1>[N:4]1[CH:3]=[C:2]([C:16](=[O:18])[CH3:17])[N:6]2[CH2:7][CH2:8][CH2:9][CH2:10][C:5]=12
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참가 물질

5

반응물 3

HCID 522689Potassium FluorideHCID 619414Stannane, tributyl(1-ethoxyethenyl)-HCID 100356983-bromo-5H,6H,7H,8H-imidazo[1,2-a]pyridine

생성물 1

HCID 686856991-(5,6,7,8-Tetrahydroimidazo[1,2-a]pyridin-3-yl)ethanone

시약·촉매·용매 1

HCID 1140Toluene용매

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온도
120 °C

실험 절차

142 mg of the 3-bromo-5,6,7,8-tetrahydroimidazo[1,2-a]pyridine [44-2] was dissolved in 2.5 mL of toluene, 81.6 mg of tetrakis triphenylphosphine palladium (0) and 477 μL of tributyl(1-ethoxyvinyl)tin were added, and the mixture was stirred overnight at 120° C. The reaction mixture was cooled back to room temperature to add 10% aqueous solution of potassium fluoride, and extracted with ethyl acetate. The organic layer was washed with 10% aqueous solution of potassium fluoride and with saturated brine in the subsequent order, and then was dried over anhydrous sodium sulfate. The insolubles were filtered, the filtrate was concentrated under reduced pressure, and then the purification by silica gel column chromatography was carried out. The obtained compound was dissolved in 2 mL of chloroform, 200 μL of 10% hydrochloric acid-methanol solution was added, and the mixture was stirred for 40 minutes. The liquid was basified by adding a saturated aqueous solution of sodium hydrogen carbonate, and was extracted with chloroform. The organic layer was washed with saturated brine, and then dried over anhydrous sodium sulfate. The insolubles were filtered, the filtrate was concentrated under reduced pressure, and the obtained residue was purified by preparative thin-layer chromatography to obtain 62.2 mg of 1-(5,6,7,8-tetrahydroimidazo[1,2-a]pyridin-3-yl)ethanone [44-3] as a pale yellow oily product.

후처리

  1. temperatureThe reaction mixture was cooled back to room temperature
  2. extractionextracted with ethyl acetate
  3. washThe organic layer was washed with 10% aqueous solution of potassium fluoride and with saturated brine in the subsequent order
  4. dry with materialwas dried over anhydrous sodium sulfate
  5. filtrationThe insolubles were filtered
  6. concentrationthe filtrate was concentrated under reduced pressure
  7. customthe purification by silica gel column chromatography
  8. dissolutionThe obtained compound was dissolved in 2 mL of chloroform
  9. addition200 μL of 10% hydrochloric acid-methanol solution was added
  10. stirringthe mixture was stirred for 40 minutes
  11. additionby adding a saturated aqueous solution of sodium hydrogen carbonate
  12. extractionwas extracted with chloroform
  13. washThe organic layer was washed with saturated brine
  14. dry with materialdried over anhydrous sodium sulfate
  15. filtrationThe insolubles were filtered
  16. concentrationthe filtrate was concentrated under reduced pressure
  17. customthe obtained residue was purified by preparative thin-layer chromatography

출처 및 근거

ORD 기록
ord-418da12252c04ef5841298e232ebcf1c
출처 데이터셋
uspto-grants-2010_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07718801B2

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