Reaktion #2095

ord-c12104568b5442eda2e049aa7fbffb8a

Lösungsmittel

Reaktionsbedingungen

Temperatur
70°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    FiltrationThe product was then filtered
  2. 2
    Einengenthe filtrate was concentrated under reduced pressure
  3. 3
    Sonstigethe oily residue which remained was chromatographed on a silica gel column (eluent: ethyl acetate/methanol 10:1)

Vorschrift

8 g (0.022 mol) of 7-(4-diethylphosphonobutyl)-3-methylxanthine (according to Example 24) were suspended in 100 ml of DMF, treated with 6.13 g (0.027 mol) of diethyl 4-chlorobutanephosphonate and 3.7 g (0.028 mol) of activated potassium carbonate and heated at 70° C. for 4 hours. The product was then filtered, the filtrate was concentrated under reduced pressure and the oily residue which remained was chromatographed on a silica gel column (eluent: ethyl acetate/methanol 10:1).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05728686uspto-grants-1998_03