Reaktion #2120

ord-1ccbe3ff71f04729a89ed7db3a53f3b8

Lösungsmittel

Reaktionsbedingungen

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

Aufarbeitung

  1. 1
    FiltrationThe solid was filtered off
  2. 2
    Einengenthe filtrate was concentrated under reduced pressure
  3. 3
    Filtrationfiltered again
  4. 4
    Sonstigecrystallized from diisopropyl ether

Vorschrift

9 g (0.04 mol) of 7-methoxyethyl-3-methylxanthine were suspended in 100 ml of DMF, treated with 11 g (0.048 mol) of diethyl 4-chlorobutane-phosphonate and 10 g (0.064 mol) of activated potassium carbonate and heated at 70° C. for 4 hours. The solid was filtered off, the filtrate was concentrated under reduced pressure and the oily residue which remained was taken up in ethyl acetate, filtered again and crystallized from diisopropyl ether.

Quelle

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