Reaktion #565816

Reaktionsgleichung

4-Fluorobenzoic acid methyl ester

1-benzyl-piperazine

potassium carbonate

→

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

Lösungsmittel

acetonitrile

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturunder reflux for 6 days
2. 2
   SonstigeAfter evaporation of the solvent
3. 3
   workup.DISSOLUTIONthe residue is dissolved in water
4. 4
   Extraktionextracted three times with diethylether
5. 5
   TrocknenThe extract is dried over sodium sulfate
6. 6
   Sonstigeevaporated
7. 7
   SonstigeThe residue is purified by flash chromatographic on silica gel with (CH2Cl2 first
8. 8
   workup.ADDITIONThe product containing fractions
9. 9
   Sonstigeevaporated
10. 10
    Filtrationthe solid filtered of and
11. 11
    Sonstigedried (vacuum)
12. 12
    SonstigeA powder with mp. 105-107° C. is obtained

Vorschrift

4-Fluorobenzoic acid methyl ester (200 mmol), 1-benzyl-piperazine (300 mmol), and potassium carbonate (300 mmol) are suspended in acetonitrile (400 ml) and stirred under reflux for 6 days. After evaporation of the solvent, the residue is dissolved in water and extracted three times with diethylether. The extract is dried over sodium sulfate and evaporated. The residue is purified by flash chromatographic on silica gel with (CH2Cl2 first, then CH2Cl2/MeOH=15:1) as mobile phase. The product containing fractions are combined and evaporated. The residue is suspended in diethylether/pentane and the solid filtered of and dried (vacuum). A powder with mp. 105-107° C. is obtained.

Quelle