Reaktion #669062

ord-08fb5b5271d448cf9530bbfd9ee00e0c

Lösungsmittel

Reaktionsbedingungen

Temperatur
90°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Einengenconcentrated for removement of dimethylformamide
  2. 2
    Extraktionextracted with dichloromethane
  3. 3
    Sonstigedried
  4. 4
    Filtrationfiltered
  5. 5
    Sonstigeseparated by column chromatography

Vorschrift

A mixture of sodium bicarbonate (0.10 g, 1.2 mmol) and lithium iodide (13 mg, 0.1 mmol) were added to dimethylformamide solution (10 ml) of 5-ethyl-6-(3,5-dimethylbenzoyl)-2,4-pyrimidinedione (0.27 g, 1.0 mmol) and 2-(cyclopent-1-en-1-yl)ethyl toluenesulfonate (0.27 g, 1.0 mmol). And then, the reaction mixture was stirred at 90° C. for overnight, concentrated for removement of dimethylformamide, extracted with dichloromethane, dried, filtered and separated by column chromatography to give a desirable product as a white solid (148 mg).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05922727uspto-grants-1999_07