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0 °C

To a stirred suspension of 1-(2-tert-butyl-4-methylphenyl)piperazine dihydrochloride (Reference Example 10, 0.300 g, 0.98 mmol) and triethylamine (548 μl, 3.93 mmol) in THF (10 mL) stirring at 0° C. was added ethyl chloro(oxo)acetate (0.175 mg, 1.28 mmol). The mixture was warmed to room temperature. After 3 days the reaction mixture was poured into water and extracted with ethyl acetate. The organic layer was washed with brine, dried over MgSO4, and the solvent was evaporated under reduced pressure to give the crude product. The product was purified by flash column chromatography (silica gel, n-hexane/ethyl acetate=90:10 to 50:50) to provide ethyl [4-(2-tert-butyl-4-methylphenyl)piperazin-1-yl](oxo)acetate (0.233 g, 71%) as a white solid.

1. temperatureThe mixture was warmed to room temperature
2. extractionextracted with ethyl acetate
3. washThe organic layer was washed with brine
4. dry with materialdried over MgSO4
5. customthe solvent was evaporated under reduced pressure
6. customto give the crude product
7. customThe product was purified by flash column chromatography (silica gel, n-hexane/ethyl acetate=90:10 to 50:50)