Reaktion #565803

Reaktionsgleichung

4-Fluorobenzoic acid methyl ester

1-methyl-piperazine

potassium carbonate

→

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

Lösungsmittel

acetonitrile

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturunder reflux for three days
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
   SonstigeThe residue is purified by flash chromatography on silica gel with (CH2Cl2/MeOH=95:5) as mobile phase
8. 8
   workup.ADDITIONThe product containing fractions
9. 9
   Sonstigeevaporated
10. 10
    Filtrationthe solid filtered of and
11. 11
    Sonstigedried (vacuum)
12. 12
    SonstigeA pale yellow powder with mp. 117-119° C., Rf=0.20 (CH2Cl2/MeOH=95:5) is obtained

Vorschrift

4-Fluorobenzoic acid methyl ester (34 mmol), 1-methyl-piperazine (75 mmol) and potassium carbonate (34 mmol) are suspended in acetonitrile (30 ml) and stirred under reflux for three days. 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 purified by flash chromatography on silica gel with (CH2Cl2/MeOH=95:5) 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 pale yellow powder with mp. 117-119° C., Rf=0.20 (CH2Cl2/MeOH=95:5) is obtained.

Quelle