Reaktion #522737

ord-7a62876cb62a437184a945100505c86d

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
    workup.ADDITIONAfter the addition
  4. 4
    Temperaturthe reaction mixture is heated
  5. 5
    Temperaturat reflux
  6. 6
    workup.STIRRINGwith continued stirring for a period of about 30 minutes
  7. 7
    FiltrationAfter this time the reaction mixture is filtered

Vorschrift

Tetrahydro-1-(5-t-butyl-1,3,4-thiadiazol-2-yl)- 3-methyl-6-hydroxy-2(1H)-pyrimidinone (0.05 mole), triethylamine (0.06 mole) and benzene (50 ml) are charged into a glass reaction vessel equipped with a mechanical stirrer, thermometer and reflux condenser. Propynoyl chloride (0.05 mole) is then added dropwise with stirring. After the addition is completed, the reaction mixture is heated at reflux with continued stirring for a period of about 30 minutes. After this time the reaction mixture is filtered and the filtrate is stripped of solvent under reduced pressure to yield the desired product tetrahydro-1-(5-t-butyl-1,3,4-thiadiazol- 2-yl)-3-methyl-6-propynoyloxy-2(1H)-pyrimidinone as the residue.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04006009uspto-grants-1977_02