反应详情

1 mmol of 2,4-dichlorophenacyl chloride in DMF was added drop wise to 1. mmol of tert-butyl piperazinecarboxylate and 1.2 mmol Cs2CO3 in DMF at room temperature for fourteen hours. The reaction mixture was concentrated in vacuo and diluted with water and ethyl acetate. The solution was extracted three times with ethyl acetate, dried over sodium sulfate, and purified by column chromatography eluting with 50% ethylacetate and 50% hexane to obtain tert-butyl 4-[2-(2,4-dichlorophenyl)-2-oxoethyl]piperazinecarboxylate.

1. concentrationThe reaction mixture was concentrated in vacuo
2. additiondiluted with water and ethyl acetate
3. extractionThe solution was extracted three times with ethyl acetate
4. dry with materialdried over sodium sulfate
5. custompurified by column chromatography
6. washeluting with 50% ethylacetate and 50% hexane