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Piperidine → 2-(4-fluorophenyl)-5-[4-(methylthio)phenyl]4-piperidino-3(2H)-pyridazinone

HRID 381931
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 381931
[NH:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[Li]CCCC.[F:12][C:13]1[CH:18]=[CH:17][C:16]([N:19]2[C:24](=[O:25])[C:23](OC)=[C:22]([C:28]3[CH:33]=[CH:32][C:31]([S:34][CH3:35])=[CH:30][CH:29]=3)[CH:21]=[N:20]2)=[CH:15][CH:14]=1.[NH2-].[Li+]>C1(C)C=CC=CC=1>[F:12][C:13]1[CH:18]=[CH:17][C:16]([N:19]2[C:24](=[O:25])[C:23]([N:1]3[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]3)=[C:22]([C:28]3[CH:29]=[CH:30][C:31]([S:34][CH3:35])=[CH:32][CH:33]=3)[CH:21]=[N:20]2)=[CH:15][CH:14]=1
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Komponenten

6

Edukt 4

HCID 8082PiperidineHCID 24532Lithium amideHCID 219341922-(4-Fluorophenyl)-4-methoxy-5-[4-(methylthio)phenyl]-3(2H)-pyridazinoneHCID 178418339Butyllithium

Produkt 1

HCID 219341832-(4-fluorophenyl)-5-[4-(methylthio)phenyl]4-piperidino-3(2H)-pyridazinoneAusbeute 95,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel2×

Reaktionsbedingungen

Temperatur
-78 °C

Versuchsvorschrift

To a slightly heterogeneous solution of piperidine (99.7 mg, 1.17 mmol) and toluene (8 mL) cooled to −78° C. was slowly added dropwise an n-BuLi solution (0.235 mL, 0.59 mmol, 2.5 M in hexanes). After stirring at −78° C. for 10 minutes, the cooling bath was removed and the mixture stirred an additional 1 hour at 23° C. The 2-(4-fluorophenyl)-4-methoxy-5-[4-(methylthio)phenyl]-3(2H)-pyridazinone (400 mg, 1.17 mmol) was dissolved in portions in toluene (3×6-7 mL aliquots) with a heat gun and cooled to 0° C. prior to transfer via syringe to the lithium amide solution (cooled to −78° C.). The addition was made slowly along the interior wall of the reaction vessel. This reaction mixture was stirred overnight, slowly warming to 23° C. as the cooling bath evaporated. The reaction was quenched with water and diluted with a large excess of ethyl acetate. The layers were separated, and the ethyl acetate layer washed with additional water and brine and dried over MgSO4, filtered, and concentrated in vacuo. The residue was chromatographed (flash silica gel, ethyl acetate/hexanes 1:2) to provide 440 mg (95%) of 2-(4-fluorophenyl)-5-[4-(methylthio)phenyl]4-piperidino-3(2H)-pyridazinone.

Aufarbeitung

  1. customthe cooling bath was removed
  2. stirringthe mixture stirred an additional 1 hour at 23° C
  3. temperaturecooled to 0° C.
  4. additionThe addition
  5. stirringThis reaction mixture was stirred overnight
  6. temperatureslowly warming to 23° C. as the cooling bath
  7. customevaporated
  8. customThe reaction was quenched with water
  9. additiondiluted with a large excess of ethyl acetate
  10. customThe layers were separated
  11. washthe ethyl acetate layer washed with additional water and brine
  12. dry with materialdried over MgSO4
  13. filtrationfiltered
  14. concentrationconcentrated in vacuo
  15. customThe residue was chromatographed (flash silica gel, ethyl acetate/hexanes 1:2)

Quellen und Nachweise

ORD-Eintrag
ord-a803bcd9f6ab4531b36f1d8725338b99
Quelldatensatz
uspto-grants-2001_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06307047B1

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