Reaktion #2318394

Reaktionsgleichung

7-trifluoromethyl-1,2,3,4-tetrahydro-1-oxo-2-naphthaleneacetic acid

phenylhydrazine

→

2-phenyl-9-trifluoromethyl-4,4a,5,6-tetrahydrobenzo[h]cinnolin-3(2H)-one

Lösungsmittel

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturis refluxed
2. 2
   Temperaturunder heating for 10 hours
3. 3
   workup.DISTILLATIONthe ethanol is distilled off
4. 4
   workup.ADDITIONTo the residue is added acetic acid
5. 5
   Temperaturthe mixture is refluxed
6. 6
   Temperaturunder heating for 7 hours
7. 7
   workup.DISTILLATIONAfter the acetic acid is distilled off
8. 8
   Extraktionthe residue is extracted with chloroform
9. 9
   Waschenthe extract is washed with water
10. 10
    Trocknendried over magnesium sulfate anhydride
11. 11
    workup.DISTILLATIONThe chloroform is distilled off

Vorschrift

After a mixture of 7-trifluoromethyl-1,2,3,4-tetrahydro-1-oxo-2-naphthaleneacetic acid and phenylhydrazine in ethanol is refluxed under heating for 10 hours, the ethanol is distilled off. To the residue is added acetic acid and the mixture is refluxed under heating for 7 hours. After the acetic acid is distilled off, the residue is extracted with chloroform and the extract is washed with water and dried over magnesium sulfate anhydride. The chloroform is distilled off to give 2-phenyl-9-trifluoromethyl-4,4a,5,6-tetrahydrobenzo[h]cinnolin-3(2H)-one.

Quelle