Methane → HCID 178519944, Verbindung

HRID 356291

Reaktionsgleichung

Reaktionsgleichung von HRID 356291
C([O:5][CH2:6][CH3:7])(=O)CO.[NH2:8][C:9]1[C:14]([NH2:15])=[CH:13][N:12]=[CH:11][N:10]=1.C>>[OH:5][CH2:6][C:7]1[NH:8][C:9]2[N:10]=[CH:11][N:12]=[CH:13][C:14]=2[N:15]=1

Komponenten

4

Edukt 3

HCID 297MethaneHCID 12184Ethyl GlycolateHCID 837034,5-Diaminopyrimidine

Produkt 1

HCID 178519944HCID 178519944, VerbindungAusbeute 58,5 %

Reaktionsbedingungen

Temperatur
140 °C

Versuchsvorschrift

8.58 g of ethyl glycolate were added to 2.27 g of 4,5-diaminopyrimidine, and the resulting mixture was stirred at 140° C. for 2 hours. At the end of this time, the reaction mixture was freed from ethyl glycolate by distillation under reduced pressure. The residue thus obtained was decolorized by activated charcoal and crystallized by trituration with ethanol, to give 1.81 g of the title compound having Rf=0.27 (on silica gel thin layer chromatography using a 10:1 by volume mixture of ethyl acetate and methanol as the developing solvent).

Aufarbeitung

  1. distillationAt the end of this time, the reaction mixture was freed from ethyl glycolate by distillation under reduced pressure
  2. customThe residue thus obtained
  3. customcrystallized by trituration with ethanol

Quellen und Nachweise

ORD-Eintrag
ord-587a2a1899d046029fd55ec504cbd6b7
Quelldatensatz
uspto-grants-1998_11
Patentnummer
US05834501

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