Formic Acid → 2,4,6-Triamino-5-formylaminopyrimidine hydrate

HRID 265617

Reaktionsgleichung

Reaktionsgleichung von HRID 265617
[NH2:1][C:2]1[N:7]=[C:6]([NH2:8])[C:5]([N:9]=[O:10])=[C:4]([NH2:11])[N:3]=1.[CH:12]([O-])=[O:13].[NH4+].C(O)=O>O.[Pd]>[OH2:10].[NH2:1][C:2]1[N:7]=[C:6]([NH2:8])[C:5]([NH:9][CH:12]=[O:13])=[C:4]([NH2:11])[N:3]=1

Komponenten

6

Edukt 3

HCID 284Formic AcidHCID 705045-Nitroso-2,4,6-pyrimidinetriamineHCID 2723923Ammonium formate

Produkt 1

HCID 190345712,4,6-Triamino-5-formylaminopyrimidine hydrate

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23938PalladiumKatalysatorHCID 962WaterLösungsmittel

Versuchsvorschrift

A suspension of 7.9 g (0.05 mol) of 2,4,6-triamino-5-nitrosopyrimidine in 50 ml of water was mixed with 3.25 g (0.05 mol) of ammonium formate, 13.9 g (0.3 mol) of formic acid and 0.5 g of the palladium catalyst according to Example 1. This mixture was heated for 4 hours to 100° C. After cooling, the catalyst was filtered off, the filtrate concentrated to about 25 ml and neutralised with about 10 ml of 25% aqueous sodium hydroxide solution to pH 7.5. A crystal slurry thereby resulted which was filtered off with suction. In this way, there were obtained 8.1 g (87% of theory) of pale beige crystals of 2,4,6-triamino-5-formylaminopyrimidine hydrate.

Aufarbeitung

  1. temperatureThis mixture was heated for 4 hours to 100° C
  2. temperatureAfter cooling
  3. filtrationthe catalyst was filtered off
  4. concentrationthe filtrate concentrated to about 25 ml and neutralised with about 10 ml of 25% aqueous sodium hydroxide solution to pH 7.5
  5. customA crystal slurry thereby resulted which
  6. filtrationwas filtered off with suction

Quellen und Nachweise

ORD-Eintrag
ord-22d8c7d4ff7841bc8f18a63ea30d28c0
Quelldatensatz
uspto-grants-1997_07
Patentnummer
US05648490

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