Diethyl Ether → 6-Hydroxy-8-methyl-3-(2-methylpropyl)-3,9-dihydro-2H-purin-2-one

HRID 464610Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 464610
[NH2:1][C:2]1[C:3](=[O:14])[NH:4][C:5](=[O:13])[N:6]([CH2:9][CH:10]([CH3:12])[CH3:11])[C:7]=1[NH2:8].C(Cl)(Cl)Cl.[CH3:19][CH2:20]OCC>C(O)(=O)C>[CH3:19][C:20]1[NH:1][C:2]2[C:3](=[O:14])[NH:4][C:5](=[O:13])[N:6]([CH2:9][CH:10]([CH3:11])[CH3:12])[C:7]=2[N:8]=1

Komponenten

5

Edukt 3

HCID 3283Diethyl EtherHCID 6212ChloroformHCID 105841095,6-Diamino-1-(2-methylpropyl)-1,2,3,4-tetrahydropyrimidine-2,4-dione

Produkt 1

HCID 30590036-Hydroxy-8-methyl-3-(2-methylpropyl)-3,9-dihydro-2H-purin-2-one

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Versuchsvorschrift

10 g of 5,6-diamino-1-(2-methylpropyl)-2,4-(1H,3H)-pyrimidine dione was refluxed in 50 ml of acetic acid for 1 hour. 30 ml of chloroform was added and ether was then added slowly. The received crystals were filtered off. Yield 10.8 g. The amide was refluxed in 30 ml of 2N NaOH for 1 hour and then neutralized with 5N HCl. The crystals were filtered off and recrystallized from 50 ml of acetic acid. Yield 3.3 g. NMR (see Table I).

Aufarbeitung

  1. filtrationThe received crystals were filtered off
  2. temperatureThe amide was refluxed in 30 ml of 2N NaOH for 1 hour
  3. filtrationThe crystals were filtered off
  4. customrecrystallized from 50 ml of acetic acid

Quellen und Nachweise

ORD-Eintrag
ord-a19745e9fd3e418d8095cdd4c94ba264
Quelldatensatz
uspto-grants-1985_10
Patentnummer
US04548818

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