反应详情

A mixture of the 1-[2-(4-t-butylcyclohexyl)phenyl]piperazine (92 mg, 0.306 mmol) produced in Example (10a), triethylamine (0.085 mL, 0.612 mmol) and dichloromethane (2 mL) was cooled in an ice bath and stirred. Ethyl chloroformate (0.032 mL, 0.337 mmol) was added to the mixture, followed by stirring for 2 hours under the same conditions. Saturated aqueous solution of sodium hydrogencarbonate was added to the reaction mixture and extraction was performed with ethyl acetate. The separated organic layer was washed with water and brine in that order and then dried over anhydrous sodium sulfate. The desiccant was filtered off and the filtrate was concentrated under reduced pressure. The resultant residue was purified by NH silica gel column chromatography (ethyl acetate/hexane) to give 100 mg of the title compound as a colorless oil, as a mixture of diastereomers at the position of t-butylcyclohexyl.

1. temperaturewas cooled in an ice bath
2. stirringby stirring for 2 hours under the same conditions
3. washThe separated organic layer was washed with water and brine in that order
4. dry with materialdried over anhydrous sodium sulfate
5. filtrationThe desiccant was filtered off
6. concentrationthe filtrate was concentrated under reduced pressure
7. customThe resultant residue was purified by NH silica gel column chromatography (ethyl acetate/hexane)