Phosphorus oxychloride → 2-Chloro-3-(4-methoxyphenyl)pyrazine

HRID 267930Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 267930
O[C:2]1[C:7]([C:8]2[CH:13]=[CH:12][C:11]([O:14][CH3:15])=[CH:10][CH:9]=2)=[N:6][CH:5]=[CH:4][N:3]=1.P(Cl)(Cl)([Cl:18])=O>>[Cl:18][C:2]1[C:7]([C:8]2[CH:13]=[CH:12][C:11]([O:14][CH3:15])=[CH:10][CH:9]=2)=[N:6][CH:5]=[CH:4][N:3]=1

Komponenten

3

Edukt 2

HCID 24813Phosphorus oxychlorideHCID 1784889683-(4-Methoxyphenyl)pyrazin-2(1H)-one

Produkt 1

HCID 131998882-Chloro-3-(4-methoxyphenyl)pyrazine

Versuchsvorschrift

The 2-hydroxy-3-p-methoxyphenylpyrazine is refluxed (120°-130°C) with excess phosphorus oxychloride under stirring for 3-5 hours. The solution is evaporated to dryness at 50°C in vacuo, cooled, ice is added, then treated with 10% sodium hydroxide solution, extracted with a suitable solvent such as diethyl ether, the ethereal solution washed with water and evaporated. The crude product is crystallized from a suitable solvent such as ethanol to give 2-chloro-3-p-methoxyphenylpyrazine.

Aufarbeitung

  1. customThe solution is evaporated to dryness at 50°C in vacuo
  2. temperaturecooled
  3. additionice is added
  4. additiontreated with 10% sodium hydroxide solution
  5. extractionextracted with a suitable solvent such as diethyl ether
  6. washthe ethereal solution washed with water
  7. customevaporated
  8. customThe crude product is crystallized from a suitable solvent such as ethanol

Quellen und Nachweise

ORD-Eintrag
ord-43b7ff0974b84d5396923adc3e3a2dd3
Quelldatensatz
uspto-grants-1976_03
Patentnummer
US03946009

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