反应详情

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.

1. temperatureunder reflux overnight
2. customAfter evaporation of the solvent
3. dissolutionthe residue is dissolved in water
4. extractionextracted three times with ethyl acetate
5. dry with materialThe extract is dried over sodium sulfate
6. customevaporated
7. filtrationthe solid filtered of and
8. customdried (vacuum)
9. customA brownish powder with mp. 102-104° C., Rf=0.22 (CH2Cl2MeOH=95:5) is obtained