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温度

0 °C

A mixture of 4-[2-(4,4-diethylcyclohexyl)phenyl]piperazine-1-carboxylic acid t-butyl ester (1.12 g, 2.80 mmol) produced in Example (38b), trifluoroacetic acid (10 mL, 130 mmol) and dichloromethane (10 mL) was stirred for 10 minutes at an external temperature of 0° C., and the temperature was raised to room temperature followed by stirring for 30 minutes. Potassium carbonate was then gradually added to the reaction mixture to make the mixture basic. Then, ethyl acetate and water were added and extraction was performed with ethyl acetate. The separated organic layer was washed with brine and dried over anhydrous magnesium sulfate. The desiccant was filtered off and then the filtrate was concentrated under reduced pressure. The resultant residue was purified by silica gel column chromatography (dichloromethane/methanol) to give 912 mg of the title compound as a white solid.

1. temperaturethe temperature was raised to room temperature
2. stirringby stirring for 30 minutes
3. extractionextraction
4. washThe separated organic layer was washed with brine
5. dry with materialdried over anhydrous magnesium sulfate
6. filtrationThe desiccant was filtered off
7. concentrationthe filtrate was concentrated under reduced pressure
8. customThe resultant residue was purified by silica gel column chromatography (dichloromethane/methanol)