反应详情

A suspension of 1-(2-tert-butyl-4-methylphenyl)piperazine dihydrochloride (Reference Example 10, 0.300 g, 0.98 mmol), 3-ethoxy-3-oxopropanoic acid (0.169 g, 1.28 mmol), EDCI (0.245 g, 1.28 mmol), HOBt (0.173 g, 1.28 mmol) and triethylamine (411 μl, 2.95 mmol) in acetonitrile (10 mL) was stirred at room temperature for 3 days. The reaction mixture was poured into saturated sodium hydrogen carbonate solution and extracted with ethyl acetate. The organic layer was washed with saturated sodium hydrogen carbonate solution and brine, dried over MgSO4, and the solvent was evaporated in vacuum to give the crude product. The product was purified by flash column chromatography (silica gel, n-hexane/ethyl acetate=90:20 to 50:50) to provide ethyl 3-[4-(2-tert-butyl-4-methylphenyl)piperazin-1-yl]-3-oxopropanoate (0.234 g, 69%) as a colorless gum.

1. extractionextracted with ethyl acetate
2. washThe organic layer was washed with saturated sodium hydrogen carbonate solution and brine
3. dry with materialdried over MgSO4
4. customthe solvent was evaporated in vacuum
5. customto give the crude product
6. customThe product was purified by flash column chromatography (silica gel, n-hexane/ethyl acetate=90:20 to 50:50)