反应详情

Charge a reaction vessel with N-tert-butoxycarbonylpiperazine (1.600 g, 8.590 mmol), potassium carbonate (3.56 g, 25.77 mmol), sodium iodide (catalytic) (10 mg, 66.7 mmol), 1,4-dioxane (20 mL), and 1-bromo-2-fluoroethane (704.0 μL, 9.45 mmol). Heat the mixture with stirring at reflux temperature overnight. Upon reaction completion, cool to room temperature and concentrate under reduced pressure. Partition the resulting residue with ethyl acetate and water. Separate the organic layer and dry over anhydrous sodium sulfate, filter, and concentrate under reduced pressure to afford pure 4-(2-fluoro-ethyl)-piperazine-1-carboxylic acid tert-butyl ester. GC-MS m/z 232 (M).

1. temperatureHeat the mixture
2. temperatureat reflux temperature overnight
3. customUpon reaction completion
4. concentrationconcentrate under reduced pressure
5. customPartition the resulting residue with ethyl acetate and water
6. customSeparate the organic layer
7. dry with materialdry over anhydrous sodium sulfate
8. filtrationfilter
9. concentrationconcentrate under reduced pressure