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Benzoic Acid → 3,9-Dihydro-8-phenyl-1,3-dipropyl-1H-purine-2,6-dione

HRID 1981584
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1981584
[CH2:1]([N:4]1[C:11]([NH2:12])=[C:10]([NH2:13])[C:8](=[O:9])[N:7]([CH2:14][CH2:15][CH3:16])[C:5]1=[O:6])[CH2:2][CH3:3].[C:17](O)(=O)[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1>CO>[CH2:14]([N:7]1[C:8](=[O:9])[C:10]2[NH:13][C:17]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)=[N:12][C:11]=2[N:4]([CH2:1][CH2:2][CH3:3])[C:5]1=[O:6])[CH2:15][CH3:16]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 243Benzoic AcidHCID 50986055,6-Diamino-1,3-dipropyl-2,4(1H,3H)-pyrimidinedione

Produkt 1

HCID 1287843,9-Dihydro-8-phenyl-1,3-dipropyl-1H-purine-2,6-dioneAusbeute 77 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

1,3-dipropyl-5,6-diaminouracil (0.01 mol) was dissolved in 30 ml methanol, followed by 0.01 mol of benzoic acid and then 0.01 mol of DICD. The solution was stirred for 30 min at room temperature, filtered, and washed with a small amount of methanol. The solid was boiled for ten minutes in 2.5N KOH, filtered hot, and the liquid neutralized with concentrated HCl. The solid was collected by filtration, washed with water, redissolved in 100 ml with a minimum amount of KOH, precipitated by neutralization with HCL, filtered, washed with water, and dried. The product was identified by chemical ionization mass spectrometry and elemental analysis. Yield 77%.

Aufarbeitung

  1. filtrationfiltered
  2. washwashed with a small amount of methanol
  3. waitThe solid was boiled for ten minutes in 2.5N KOH
  4. filtrationfiltered hot
  5. filtrationThe solid was collected by filtration
  6. washwashed with water
  7. dissolutionredissolved in 100 ml with a minimum amount of KOH
  8. customprecipitated by neutralization with HCL
  9. filtrationfiltered
  10. washwashed with water
  11. customdried

Quellen und Nachweise

ORD-Eintrag
ord-0462b2d84e6240458c85d00454c61e8b
Quelldatensatz
uspto-grants-1986_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04593095

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