Potassium Carbonate → 7-(5-Hydroxy-5-methyl-6-heptynyl)-3-methylxanthine

HRID 1738800Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1738800
[CH3:1][N:2]1[C:10]2[N:9]=[CH:8][NH:7][C:6]=2[C:5](=[O:11])[NH:4][C:3]1=[O:12].Cl[CH2:14][CH2:15][CH2:16][CH2:17][C:18]([OH:22])([CH3:21])[C:19]#[CH:20].C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[OH:22][C:18]([CH3:21])([C:19]#[CH:20])[CH2:17][CH2:16][CH2:15][CH2:14][N:7]1[C:6]2[C:5](=[O:11])[NH:4][C:3](=[O:12])[N:2]([CH3:1])[C:10]=2[N:9]=[CH:8]1

Komponenten

5

Edukt 3

HCID 11430Potassium CarbonateHCID 706393-MethylxanthineHCID 131980541-Chloro-5-hydroxy-5-methyl-6-heptyne

Produkt 1

HCID 218393427-(5-Hydroxy-5-methyl-6-heptynyl)-3-methylxanthine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

33.2 g (0.2 mol) of 3-methylxanthine in 350 ml of dimethylformamide were stirred with 32.1 g (0.2 mol) of 1-chloro-5-hydroxy-5-methyl-6-heptyne from Example 1B1) in the presence of 13.8 g (0.1 mol) of potassium carbonate at 120° C. for 6 hours. The hot mixture was then filtered, evaporated to dryness under reduced pressure and taken up in ethanol and, at the boiling point, diisopropyl ether was added to cloudiness, and the mixture was left to crystallize with cooling.

Aufarbeitung

  1. filtrationThe hot mixture was then filtered
  2. customevaporated to dryness under reduced pressure
  3. additionwas added to cloudiness
  4. waitthe mixture was left
  5. customto crystallize
  6. temperaturewith cooling

Quellen und Nachweise

ORD-Eintrag
ord-e31cd4cb11704bedb52965070cc228db
Quelldatensatz
uspto-grants-1999_10
Patentnummer
US05965555

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