Reaktion #1243526

Reaktionsgleichung

sodium hydride

2-phenyl-4(3H)-quinazolinone

2-bromoethanol

→

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

Lösungsmittel

N,N-dimethylformamide

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeexothermic reaction
2. 2
   Sonstigerises to 34° C.
3. 3
   workup.ADDITIONAfter the addition
4. 4
   workup.ADDITIONare added dropwise (slightly exothermic)
5. 5
   workup.WAITfor 2 hours at 80° C.
6. 6
   Sonstigefurther overnight
7. 7
   Sonstigeat room temperature
8. 8
   TemperaturThe reaction mixture is cooled
9. 9
   workup.ADDITIONpoured onto water
10. 10
    WaschenIt is washed with water and 2,2'-oxybispropane
11. 11
    Sonstigedried in vacuo at 60° C.

Vorschrift

To a stirred mixture of 18 parts of 2-phenyl-4(3H)-quinazolinone and 225 parts of N,N-dimethylformamide are added portionwise at room temperature 3.2 parts of sodium hydride dispersion 60% (exothermic reaction: the temperature rises to 34° C.). After the addition is complete, the whole is stirred for 10 minutes whereafter 12.4 parts of 2-bromoethanol are added dropwise (slightly exothermic). Upon completion, stirring is continued first for one hour at room temperature, then for 2 hours at 80° C. and further overnight at room temperature. The reaction mixture is cooled, poured onto water and the solid product is sucked off. It is washed with water and 2,2'-oxybispropane and dried in vacuo at 60° C., yielding 15 parts of 3-(2-hydroxyethyl)-2-phenyl-4(3H)-quinazolinone.

Quelle