Reaktion #50282

ord-2c4acd62b4744dfea4477d58c9a032b0

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe solution was cooled in an ice bath
  2. 2
    SonstigeThe precipitate that formed
  3. 3
    Sonstigewas collected
  4. 4
    Temperaturrefluxed in 20 ml of dimethylformamide (DMF) for 2 h
  5. 5
    TemperaturThe reaction was cooled
  6. 6
    Sonstigethe DMF removed in vacuo
  7. 7
    workup.ADDITIONTo the resulting mixture 40 mL of water was added
  8. 8
    Sonstigethe solid collected
  9. 9
    Sonstigedried

Vorschrift

A solution of of 6,6-Dicarboethoxy-5,6,7,8-tetrahydro-2,4(1H,3H)-quinazolinedione (25 g) in 1N NaOH (350 mL) was stirred at 40° C. for 35 min. The solution was cooled in an ice bath and acidified with 35 mL of concentrated HCl. The precipitate that formed was collected and refluxed in 20 ml of dimethylformamide (DMF) for 2 h. The reaction was cooled and the DMF removed in vacuo. To the resulting mixture 40 mL of water was added and the solid collected and dried to yield 6-Carboethoxy-5,6,7,8-tetrahydro-2,4(1H ,3H)-quinazolinedione.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05426186uspto-grants-1995_06