Reaktion #522732

ord-68d4dcd6d3da4fe0bc697d8ab6f2c33f

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. α-(3,5-Dinitrophenyl)acetyl 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-[α-(3,5 -dinitrophenyl)acetyloxy] -2 (1H)-pyrimidinone as the residue.

Quelle

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