反应详情

44.7 g (240 mmol) N-(tert-butoxycarbonyl)-piperazine, 60.9 g (240 mmol) N-(2-bromoethyl)-phthalimide, 49.8 g (360 mmol) potassium carbonate and 49.5 g (330 mmol) sodium iodide are heated in 1000 ml ethyl methyl ketone for five hours under reflux. After cooling the reaction mixture and concentrated under vacuum. The residue is taken up in 700 ml chloroform and extracted twice by shaking each with 50 ml water. The organic phase is dried over sodium sulfate and the solvent is distilled off. The residue is crystallized from 110 ml methanol. Colorless crystals of MP. 136-138° C.: Yield 47.6 g (55%).

1. temperatureunder reflux
2. temperatureAfter cooling the reaction mixture
3. concentrationconcentrated under vacuum
4. extractionextracted twice
5. dry with materialThe organic phase is dried over sodium sulfate
6. distillationthe solvent is distilled off
7. customThe residue is crystallized from 110 ml methanol
8. customColorless crystals of MP. 136-138° C.