反应详情

Trifluororoacetic acid (1 mL) is added to a solution of 4-{4-[4-(4-trifluoromethyl-phenyl)-piperazin-1-yl]-butyrylamino}-piperidine-1-carboxylic acid tert-butyl ester (660 mg; 1.32 mmol, prepared in accordance with Example 74) in dichloromethane (4 mL) and the resulting mixture is stirred at room temperature. After 3 hours reaction time, the excess acid is neutralized by the addition of potassium carbonate, the mixture is filtered and the filtrate is concentrated under reduced pressure. The residue obtained is diluted in ethylacetate (20 mL) and the organic phase is extracted with water (2×10 mL). The combined aqueous phases are extracted with dichloromethane (10 mL) and diethylether (10 mL). The combined organic layers are dried over magnesium sulfate and the solvents removed under reduced pressure to afford the desired product (417 mg; 1.05 mmol).

1. customAfter 3 hours reaction time
2. filtrationthe mixture is filtered
3. concentrationthe filtrate is concentrated under reduced pressure
4. customThe residue obtained
5. extractionthe organic phase is extracted with water (2×10 mL)
6. extractionThe combined aqueous phases are extracted with dichloromethane (10 mL) and diethylether (10 mL)
7. dry with materialThe combined organic layers are dried over magnesium sulfate
8. customthe solvents removed under reduced pressure