nicotinic acid, potassium salt → 1-(1,3,7-Trimethyl-2,6-dioxo-2,3,6,7-tetrahydro-1H-purin-8-yl)ethyl pyridine-3-carboxylate

HRID 1283379

Reaktionsgleichung

Reaktionsgleichung von HRID 1283379
Cl[CH:2]([C:4]1[N:13]([CH3:14])[C:12]2[C:11](=[O:15])[N:9]([CH3:10])[C:8](=[O:16])[N:7]([CH3:17])[C:6]=2[N:5]=1)[CH3:3].[C:18]([O-:26])(=[O:25])[C:19]1[CH:24]=[CH:23][CH:22]=[N:21][CH:20]=1.[K+]>CN(C)C=O>[C:18]([O:26][CH:2]([C:4]1[N:13]([CH3:14])[C:12]2[C:11](=[O:15])[N:9]([CH3:10])[C:8](=[O:16])[N:7]([CH3:17])[C:6]=2[N:5]=1)[CH3:3])(=[O:25])[C:19]1[CH:24]=[CH:23][CH:22]=[N:21][CH:20]=1

Komponenten

4

Edukt 2

HCID 23668574nicotinic acid, potassium saltHCID 681383658-alpha-Chloroethylcaffeine

Produkt 1

HCID 30436851-(1,3,7-Trimethyl-2,6-dioxo-2,3,6,7-tetrahydro-1H-purin-8-yl)ethyl pyridine-3-carboxylate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

2.57 g of 8-α-chloroethylcaffeine are dissolved in 25 ml of anhydrous dimethylformamide, to which 2.98 g of dry potassium nicotinate are added. The mixture is heated under shaking at 100° C for 1 hour, then filtered off and the filtrate evaporated under reduced pressure. The residue, after washing with water, gives 3.1 g of slightly crude product which is purified by crystallization from 95% ethanol : m.p. (EtOH) 160° C. The monohydrochloride melts at 200°-210° C.

Aufarbeitung

  1. additionare added
  2. temperatureThe mixture is heated
  3. filtrationfiltered off
  4. customthe filtrate evaporated under reduced pressure
  5. washThe residue, after washing with water
  6. customgives 3.1 g of slightly crude product which
  7. customis purified by crystallization from 95% ethanol
  8. customm.p. (EtOH) 160° C

Quellen und Nachweise

ORD-Eintrag
ord-7614fee6f4414fc9aa036d4be747f38e
Quelldatensatz
uspto-grants-1976_08
Patentnummer
US03975389

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