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Gamma-Butyrolactone → 4-Hydroxy-1-(3-pyridyl)-1-butanone

HRID 484021
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 484021
Br[C:2]1[CH:3]=[N:4][CH:5]=[CH:6][CH:7]=1.CCCCCC.C([Li])CCC.[C:19]1(=[O:24])[O:23][CH2:22][CH2:21][CH2:20]1>CCOCC>[N:4]1[CH:5]=[CH:6][CH:7]=[C:2]([C:22](=[O:23])[CH2:21][CH2:20][CH2:19][OH:24])[CH:3]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 7302Gamma-ButyrolactoneHCID 122863-BromopyridineHCID 178418244HCID 178418244, Verbindung

Produkt 1

HCID 1078194-Hydroxy-1-(3-pyridyl)-1-butanoneAusbeute 77 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3283Diethyl EtherLösungsmittel2×

Versuchsvorschrift

A solution of 10.0 g (63.3 mmol) of 3-bromopyridine in 100 ml of ether was cooled to -78° C., to which 40 ml (64 mmol) of 1.6M n-butyllithium hexane solution was added dropwise with stirring. After completion of the addition, the mixture was stirred for further 15 minutes, to which the solution of 5.45 g (63.3 mmol) of γ-butyrolactone in 15 ml of ether was added dropwise, and stirred for further 1 hour at -78° C.-room temperature. To the reaction mixture an aqueous solution of ammonium chloride, and the resultant substance was extracted with ethyl acetate. The extract was washed with water and dried, and the solvent was evaporated off. The residue was purified with silica gel column chromatography (CHCl3 -MeOH (9:1)) and recrystallized from ethyl acetate-isopropyl ether, to give 8.0 g (77%) of 4-(3-pyridyl)-4-oxobutanol. m.p. 36°-37° C.

Aufarbeitung

  1. additionwas added dropwise
  2. additionAfter completion of the addition
  3. additionwas added dropwise
  4. stirringstirred for further 1 hour at -78° C.-room temperature
  5. extractionTo the reaction mixture an aqueous solution of ammonium chloride, and the resultant substance was extracted with ethyl acetate
  6. washThe extract was washed with water
  7. customdried
  8. customthe solvent was evaporated off
  9. customThe residue was purified with silica gel column chromatography (CHCl3 -MeOH (9:1))
  10. customrecrystallized from ethyl acetate-isopropyl ether

Quellen und Nachweise

ORD-Eintrag
ord-f937b5bb59154b42b8e4442473ad9802
Quelldatensatz
uspto-grants-1993_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05229385

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