Water → 139393-89-8

HRID 273685

Reaktionsgleichung

Reaktionsgleichung von HRID 273685
[C:1]([C:3]1[C:4](=O)[NH:5][C:6]([CH3:11])=[C:7]([CH2:9][CH3:10])[CH:8]=1)#[N:2].P(Cl)(Cl)(Cl)(Cl)[Cl:14].O>CCCCCC>[Cl:14][C:4]1[C:3]([C:1]#[N:2])=[CH:8][C:7]([CH2:9][CH3:10])=[C:6]([CH3:11])[N:5]=1

Komponenten

5

Edukt 3

HCID 962WaterHCID 24819Phosphorus pentachlorideHCID 102411095-Ethyl-6-methyl-2-oxo-1,2-dihydropyridine-3-carbonitrile

Produkt 1

HCID 10103778139393-89-8Ausbeute 61,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8058HexaneLösungsmittel

Versuchsvorschrift

3-Cyano-5-ethyl-6-methyl-2-(1H)-pyridinone (22.9 g, 0.141 mol) and phosphorus pentachloride (33.1 g, 0.159 mol) were intimately mixed and heated at 110°-120° C. for one hour. The liquified solids were poured onto crushed ice and water and the semi-solid was extracted into chloroform. This extract was washed with water, saturated aqueous NaHCO3, dried (Na2SO4), filtered and evaporated. This amber oil was dissolved in hexane and the insoluble material was removed when filtered through a pad of charcoal. Removal of the solvent gave a light yellow oil which solidified (17.7 g). Trituration of this solid with cold hexane yielded 15.6 g (61%) of pure product, m.p. 63°-64° C.

Aufarbeitung

  1. temperatureheated at 110°-120° C. for one hour
  2. additionThe liquified solids were poured
  3. extractionthe semi-solid was extracted into chloroform
  4. washThis extract was washed with water, saturated aqueous NaHCO3
  5. dry with materialdried (Na2SO4)
  6. filtrationfiltered
  7. customevaporated
  8. dissolutionThis amber oil was dissolved in hexane
  9. customthe insoluble material was removed when
  10. filtrationfiltered through a pad of charcoal
  11. customRemoval of the solvent
  12. customgave a light yellow oil which

Quellen und Nachweise

ORD-Eintrag
ord-9860d2972c1749cdafeb7022841015a5
Quelldatensatz
uspto-grants-1995_02
Patentnummer
US05387512

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