Reaktion #411039

ord-2f1df5af9bd84380a8f67bba5825dc1a

Reaktionsgleichung

CCn1c(=O)[nH]c(=O)c2[nH]cnc21
3-ethylxanthine
CN(C)C=O
dimethylformamide
O=C([O-])[O-].[K+].[K+]
potassium carbonate
ClCc1ccccc1
benzyl chloride
CCn1c(=O)[nH]c(=O)c2c1ncn2Cc1ccccc1
7-Benzyl-3-ethylxanthine

Lösungsmittel

Reaktionsbedingungen

Temperatur
80°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.STIRRINGIt was then stirred at 100° C. for 2 hours
  2. 2
    Filtrationthe precipitated product was filtered on a suction
  3. 3
    Filtrationfilter
  4. 4
    Waschenwashed with water until salt-free and
  5. 5
    Sonstigedried in a vacuum
  6. 6
    Sonstigedrying oven at 100° C
  7. 7
    SonstigeIf necessary, a further purification
  8. 8
    Sonstigeby reprecipitating from 1 N sodium hydroxide solution

Vorschrift

180 g (1 mol) of 3-ethylxanthine were initially introduced into 1000 ml of dimethylformamide, the mixture was heated to 80° C. with stirring and, after the introduction of 88 g (0.64 mol) of potassium carbonate, treated dropwise with 133 g (1.05 mol) of benzyl chloride in the course of 1 hour. It was then stirred at 100° C. for 2 hours, treated with 1000 ml of water, and the precipitated product was filtered on a suction filter, washed with water until salt-free and dried in a vacuum drying oven at 100° C. If necessary, a further purification can be carried out by reprecipitating from 1 N sodium hydroxide solution using 4 N hydrochloric acid analogously to Example 1a).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06214992B1uspto-grants-2001_04