Reaktion #1335413

Reaktionsgleichung

3-(2-hydroxyethyl)-2-phenyl-4-(3H)-quinazolinone

thionyl chloride

→

3-(2-chloroethyl)-2-phenyl-4(3H)-quinazolinone

Lösungsmittel

trichloromethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturat reflux
2. 2
   SonstigeThe reaction mixture is evaporated
3. 3
   workup.ADDITIONWater is added to the residue
4. 4
   ExtraktionThe product is extracted with trichloromethane
5. 5
   WaschenThe extract is washed with water
6. 6
   Sonstigedried
7. 7
   Filtrationfiltered
8. 8
   Sonstigeevaporated
9. 9
   SonstigeThe residue is crystallized from a mixture of 2,2'-oxybispropane and petroleumether
10. 10
    FiltrationThe product is filtered off
11. 11
    Sonstigedried

Vorschrift

To a stirred mixture of 15 parts of 3-(2-hydroxyethyl)-2-phenyl-4-(3H)-quinazolinone and 375 parts of trichloromethane are added dropwise 24 parts of thionyl chloride at room temperature. Upon completion, stirring is continued for 2 hours at reflux. The reaction mixture is evaporated. Water is added to the residue and the whole is neutralized with a sodium hydrogen carbonate solution. The product is extracted with trichloromethane. The extract is washed with water, dried, filtered and evaporated. The residue is crystallized from a mixture of 2,2'-oxybispropane and petroleumether. The product is filtered off and dried, yielding 11.6 parts of 3-(2-chloroethyl)-2-phenyl-4(3H)-quinazolinone.

Quelle