Reaktion #565806

Reaktionsgleichung

4-Fluorobenzoic acid methyl ester

1-ethyl-piperazine

potassium carbonate

→

4-(4-Ethyl-piperazin-1-yl)-benzoic acid methyl ester

Lösungsmittel

dimethyl-acetamide

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturunder reflux overnight
2. 2
   SonstigeAfter evaporation of the solvent
3. 3
   workup.DISSOLUTIONthe residue is dissolved in water
4. 4
   Extraktionextracted three times with ethyl acetate
5. 5
   TrocknenThe extract is dried over sodium sulfate
6. 6
   Sonstigeevaporated
7. 7
   Filtrationthe solid filtered of and
8. 8
   Sonstigedried (vacuum)
9. 9
   SonstigeA brownish powder with mp. 102-104° C., Rf=0.22 (CH2Cl2MeOH=95:5) is obtained

Vorschrift

4-Fluorobenzoic acid methyl ester (53 mmol), 1-ethyl-piperazine (44 mmol) and potassium carbonate (44 mmol) are suspended in dimethyl-acetamide (50 ml) and stirred under reflux overnight. After evaporation of the solvent, the residue is dissolved in water and extracted three times with ethyl acetate. The extract is dried over sodium sulfate and evaporated. The residue is suspended in diethylether/pentane and the solid filtered of and dried (vacuum). A brownish powder with mp. 102-104° C., Rf=0.22 (CH2Cl2MeOH=95:5) is obtained.

Quelle