Ethanol → CH-13584

HRID 1904903Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1904903
[CH3:1][CH2:2][O-:3].[Na+].[Na].C(O)C.[CH3:9][N:10]1[C:18]2[N:17]=[CH:16][N:15]([CH2:19][C:20](=[N:22]O)[NH2:21])[C:14]=2[C:13](=[O:24])[NH:12][C:11]1=[O:25]>C(OCC)(=O)C>[CH3:9][N:10]1[C:18]2[N:17]=[CH:16][N:15]([CH2:19][C:20]3[N:22]=[C:2]([CH3:1])[O:3][N:21]=3)[C:14]=2[C:13](=[O:24])[NH:12][C:11]1=[O:25]

Komponenten

6

Edukt 4

HCID 702EthanolHCID 2723922Sodium ethoxideHCID 5360545SodiumHCID 537117962-(3-Methyl-xanthine-7-yl)acetamidoxime

Produkt 1

HCID 163975CH-13584

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

A mixture of a sodium ethylate solution prepared from 6.76 g of metallic sodium and 290 ml of anhydrous ethanol, 35 g of 2-(3-methyl-xanthine-7-yl)-acetamidoxime and 43.0 g of ethyl acetate is heated to boiling under stirring for 4 hours. The hot reaction mixture is filtered, the filtrate is evaporated in vacuo and the residue is dissolved in 200 ml of water. The pH of the solution is adjusted to 7 by adding 10% hydrochloric acid, the precipitate is filtered by suction and crystallized twice from water. Thus, 18.0 g of 3,7-dihydro-3-methyl-7-([5-methyl-1,2,4-oxadiazole-3-yl]-methyl)-1H-purine-2,6-dione are obtained, m.p.: 262°-264° C.

Aufarbeitung

  1. temperatureis heated
  2. filtrationThe hot reaction mixture is filtered
  3. customthe filtrate is evaporated in vacuo
  4. dissolutionthe residue is dissolved in 200 ml of water
  5. additionby adding 10% hydrochloric acid
  6. filtrationthe precipitate is filtered by suction
  7. customcrystallized twice from water

Quellen und Nachweise

ORD-Eintrag
ord-46c8110c31fd40d699156ebc59ba83ea
Quelldatensatz
uspto-grants-1989_06
Patentnummer
US04840949

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