Reaktion #522730

Reaktionsgleichung

Tetrahydro-1-(5-t-butyl-1,3,4-thiadiazol-2-yl)-3-methyl- 6-hydroxy-2(1H)-pyrimidinone

triethylamine

4-Trifluoromethylbenzoyl chloride

→

tetrahydro- 1-(5-t-butyl-1,3,4-thiadiazol-2-yl)-3-methyl-6-(4-trifluoromethylbenzoyloxy)-2(1H)-pyrimidinone

Lösungsmittel

benzene

Reaktionsbedingungen

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
8. 8
   Sonstigeto yield a solid residue
9. 9
   SonstigeThe residue is recrystallized

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. 4-Trifluoromethylbenzoyl 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 a solid residue. The residue is recrystallized to yield the desired product tetrahydro- 1-(5-t-butyl-1,3,4-thiadiazol-2-yl)-3-methyl-6-(4-trifluoromethylbenzoyloxy)-2(1H)-pyrimidinone.

Quelle