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

HRID 236305Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 236305
[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-5b8ad565345e41798ec6deb220cdcd93
Quelldatensatz
uspto-grants-1987_02
Patentnummer
US04644001

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