反应详情

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.

1. temperatureunder reflux for three days
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. customThe residue is purified by flash chromatography on silica gel with (CH2Cl2/MeOH=95:5) as mobile phase
8. additionThe product containing fractions
9. customevaporated
10. filtrationthe solid filtered of and
11. customdried (vacuum)
12. customA pale yellow powder with mp. 117-119° C., Rf=0.20 (CH2Cl2/MeOH=95:5) is obtained