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Chloroform → HCID 22662826, Verbindung

HRID 1005733
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1005733
N[C:2]1[N:7]=[C:6]([C:8]([NH2:10])=[O:9])[C:5]([O:11][CH3:12])=[N:4][CH:3]=1.N([O-])=O.[Na+].C(Cl)(Cl)Cl.[FH:21].N1C=CC=CC=1>>[F:21][C:2]1[N:7]=[C:6]([C:8]([NH2:10])=[O:9])[C:5]([O:11][CH3:12])=[N:4][CH:3]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 4

HCID 6212ChloroformHCID 64774Pyridine, hydrofluoride (1:1)HCID 226628026-Amino-3-methoxy-2-pyrazinecarboxamideHCID 23668193Sodium Nitrite

Produkt 1

HCID 22662826HCID 22662826, Verbindung

Reaktionsbedingungen

Temperatur
10 °C

Versuchsvorschrift

In a nitrogen atmosphere, 1.50 g of 6-amino-3-methoxy-2-pyrazinecarboxamide is dissolved in 12 mL of 70% pyridine hydrofluoride under ice-cooling. Then, 0.71 g of sodium nitrite is added thereto at −50° C., and the resulting solution is stirred at 10° C. for 1 hour. The resulting reaction mixture is stirred at ambient temperature for an additional 1 hour. Thereafter, a mixture of 50 mL of ice water and 100 mL of chloroform is added thereto and the resulting mixture is separated into layers. The organic layer is washed with saturated aqueous solution of sodium chloride and saturated aqueous solution of sodium hydrogen carbonate, and dried over anhydrous magnesium sulfate. Then, the solvent is distilled off under reduced pressure to obtain 1.29 g of 6-fluoro-3-methoxy-2-pyrazinecarboxamide.

Aufarbeitung

  1. temperaturecooling
  2. customThe resulting reaction mixture
  3. stirringis stirred at ambient temperature for an additional 1 hour
  4. additionis added
  5. customthe resulting mixture is separated into layers
  6. washThe organic layer is washed with saturated aqueous solution of sodium chloride and saturated aqueous solution of sodium hydrogen carbonate
  7. dry with materialdried over anhydrous magnesium sulfate
  8. distillationThen, the solvent is distilled off under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-eb4b04853cd140cab253dec460e39aa9
Quelldatensatz
uspto-grants-2004_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06787544B2

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