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Formaldehyde → 1,3-Dioxan-5-yl 3-pyridyl ketone

HRID 354718
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 354718
[C:1]([C:4]1[CH:5]=[N:6][CH:7]=[CH:8][CH:9]=1)(=[O:3])[CH3:2].[CH2:10]=[O:11].B(F)(F)F.C[CH2:17][O:18][CH2:19]C>C(O)(=O)C>[N:6]1[CH:7]=[CH:8][CH:9]=[C:4]([C:1]([CH:2]2[CH2:10][O:11][CH2:19][O:18][CH2:17]2)=[O:3])[CH:5]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 712FormaldehydeHCID 8000Boron trifluoride etherateHCID 95893-Acetylpyridine

Produkt 1

HCID 119709961,3-Dioxan-5-yl 3-pyridyl ketone

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Versuchsvorschrift

A 48.4 g. portion of 3-acetylpyridine was combined with 60 g. of paraformaldehyde and 200 ml. of glacial acetic acid, and to the mixture was added, dropwise with stirring, 86 g. of boron trifluoride etherate. The mixture was then heated, and was stirred under reflux for 4 hours. The reaction was cooled and the volatile materials were evaporated under vacuum to obtain 60 g. of an oily yellow solid, which was crystallized by the addition of water. The solids were separated by filtration, washed with water and dried to obtain 25 g. of the desired product, m.p. 91°-100°.

Aufarbeitung

  1. temperatureThe mixture was then heated
  2. stirringwas stirred
  3. temperatureunder reflux for 4 hours
  4. temperatureThe reaction was cooled
  5. customthe volatile materials were evaporated under vacuum
  6. customto obtain 60 g
  7. customof an oily yellow solid, which was crystallized by the addition of water
  8. customThe solids were separated by filtration
  9. washwashed with water
  10. customdried
  11. customto obtain 25 g

Quellen und Nachweise

ORD-Eintrag
ord-5e17a6783e384cc4bcdd068d1263980e
Quelldatensatz
uspto-grants-1983_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04376860

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