反应详情

1-(4-Chlorophenyl)piperazine dihydrochloride (1.88 g, 6.973 mmol) was dissolved in methylene chloride and, after slowly adding triethylamine (1.9 mL, 13.946 mmol) at 0° C., stirred for 5 minutes. After adding 3-chloropropionyl chloride (0.67 mL, 6.973 mmol), the reaction solution was stirred at room temperature. After extracting with methylene chloride, the organic layer was dried with desiccant and then filtered. The filtrate was concentrated and purified by column chromatography (EtOAc/hexane, 4:1). A target compound (1.03 g, 3.586 mmol, 51.5%) was yielded as white solid.

1. extractionAfter extracting with methylene chloride
2. customthe organic layer was dried with desiccant and
3. filtrationthen filtered
4. concentrationThe filtrate was concentrated
5. custompurified by column chromatography (EtOAc/hexane, 4:1)