Methane → HCID 86740607, Verbindung

HRID 1285179Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1285179
[N:1]1([C:12](=[O:13])[C:11]2[N:10]([CH2:14][C:15](=[N:17][OH:18])[NH2:16])[CH:9]=[N:8][C:7]=2[N:5]([CH3:6])[C:3]1=[O:4])[CH3:2].[CH3:19][O-].[Na+].[N:22]1([C:33](=[O:34])[C:32]2[N:31]([CH2:35]C(Cl)=O)[CH:30]=[N:29][C:28]=2[N:26]([CH3:27])[C:24]1=[O:25])[CH3:23].C>CN(C)C=O>[N:1]1([C:12](=[O:13])[C:11]2[N:10]([CH2:14][CH:15]3[N:16]=[C:35]([N:31]4[C:32]5[C:33](=[O:34])[N:22]([CH3:23])[C:24](=[O:25])[N:26]([CH3:27])[C:28]=5[N:29]=[CH:30]4)[O:18][N:17]3[CH3:19])[CH:9]=[N:8][C:7]=2[N:5]([CH3:6])[C:3]1=[O:4])[CH3:2]

Komponenten

6

Edukt 4

HCID 297MethaneHCID 30161851,2,3,6-Tetrahydro-1,3-dimethyl-2,6-dioxo-7H-purine-7-acetyl chlorideHCID 30574902-(Theophyllin-7-yl)-acetamidoximeHCID 10942334Sodium Methoxide

Produkt 1

HCID 86740607HCID 86740607, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel2×

Versuchsvorschrift

5.04 g. of 2-(theophyllin-7-yl)-acetamidoxime and 1.08 g. of sodium methylate are suspended in 60 cm3 dimethylformamide whereafter a solution of 5.13 g. of theophyllin-7-yl-acetyl chloride in 25 cm3 of dimethyl-formamide is added dropwise within 15 minutes. The mixture is heated for 1 hour and after adding a small amount of activated charcoal it is filtered while hot and the filtrate is evaporated at reduced pressure. The residue is dissolved in 100 cm3 0.1N sodium hydrogen carbonate solution while hot and after cooling the crystals are filtered by suction, washed with water and crystallized from 50% aqueous ethanol. Thus 6.6 g. of 3-(theophyllin-7-yl-methyl)-5-(theophylline-7-yl)-methyl-1,2,4-oxadiazole are obtained, m.p.: 271°-272° C.

Aufarbeitung

  1. temperatureThe mixture is heated for 1 hour
  2. filtrationis filtered while hot and the filtrate
  3. customis evaporated at reduced pressure
  4. dissolutionThe residue is dissolved in 100 cm3 0.1N sodium hydrogen carbonate solution while hot and
  5. temperatureafter cooling the crystals
  6. filtrationare filtered by suction
  7. washwashed with water
  8. customcrystallized from 50% aqueous ethanol

Quellen und Nachweise

ORD-Eintrag
ord-5d06331c63064c7a8648c89ff3742de7
Quelldatensatz
uspto-grants-1986_01
Patentnummer
US04565817

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