Reaktion #1502548

ord-406432225b9e44ee92b4b6cacbabb72d

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeequipped with a mechanical stirrer
  2. 2
    Temperaturthermometer and reflux condenser
  3. 3
    TemperaturThe reaction mixture is heated
  4. 4
    Temperaturat reflux for a period of about 15 minutes
  5. 5
    FiltrationThe reaction mixture is then filtered while hot and the filtrate
  6. 6
    Temperaturis cooled
  7. 7
    Sonstigeresulting in the formation of a precipitate
  8. 8
    FiltrationThe precipitate is recovered by filtration
  9. 9
    Sonstigeis dried
  10. 10
    Sonstigeis recrystallized

Vorschrift

The dimethyl acetal of 3-[1-methyl-3-(5-cycloheptyl-1,3,4-thiadiazol-2-yl)ureido]propionaldehyde (15 grams), water (400 ml) and hydrochloric acid (4 ml) are charged into a glass reaction vessel equipped with a mechanical stirrer, thermometer and reflux condenser. The reaction mixture is heated at reflux for a period of about 15 minutes. The reaction mixture is then filtered while hot and the filtrate is cooled resulting in the formation of a precipitate. The precipitate is recovered by filtration, is dried and is recrystallized to yield the desired product tetrahydro-1-(5-cycloheptyl-1,3,4-thiadiazol-2-yl)-3-methyl-6-hydroxy-2(1H)-pyrimidinone.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04004912uspto-grants-1977_01