Isoamyl Nitrite → HCID 178508438, Verbindung

HRID 2081798

Reaktionsgleichung

Reaktionsgleichung von HRID 2081798
[Cl:1][C:2]1[N:7]=[C:6]([NH2:8])[N:5]=[C:4]([NH2:9])[C:3]=1[NH2:10].[N:11](OCCC(C)C)=O>O1CCOCC1>[Cl:1][C:2]1[C:3]2[NH:10][N:11]=[N:9][C:4]=2[N:5]=[C:6]([NH2:8])[N:7]=1

Komponenten

4

Edukt 2

HCID 8053Isoamyl NitriteHCID 5005056-Chloropyrimidine-2,4,5-triamine

Produkt 1

HCID 178508438HCID 178508438, VerbindungAusbeute 78,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

A solution of 6-chloro-2,4,5-pyrimidinetriamine (10.94 g, 0.0686 mol) and isoamyl nitrite (9.20 ml, 0.0686 mol)in dioxane (500 ml, freshly purified by passage through basic alumina) was heated under nitrogen with stirring for 2 hours at 90°. The reaction mixture was cooled, treated with activated carbon, filtered, and concentrated to 150 ml. Petroleum ether (250 ml, bp 35-60°) was added. The precipitate was filtered, washed the petroleum ether (50 ml) and dried in vacuo over P2O5 at 40° for 16 hours to give 9.23 g of crude desired product which was then used in the next step.

Aufarbeitung

  1. temperaturewas heated under nitrogen
  2. temperatureThe reaction mixture was cooled
  3. additiontreated with activated carbon
  4. filtrationfiltered
  5. concentrationconcentrated to 150 ml
  6. additionPetroleum ether (250 ml, bp 35-60°) was added
  7. filtrationThe precipitate was filtered
  8. washwashed the petroleum ether (50 ml)
  9. dry with materialdried in vacuo over P2O5 at 40° for 16 hours

Quellen und Nachweise

ORD-Eintrag
ord-d6b3d8a284e94b3bab37b5e6ba0c37aa
Quelldatensatz
uspto-grants-1993_02
Patentnummer
US05185459

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