反应详情

Powdered potassium hydroxide (0.331 g, 5.90 mmol) was dissolved in EtOH (2 mL) and added to 5-[(2,2,2-trifluoroethoxy)methyl]pyridine-2-carbonitrile (Intermediate 226, 0.255 g, 1.18 mmol). The mixture was heated to 110 C for 16 h. After cooling the residue was dissolved in water (3 mL), acidified to pH 1 by adding 10% aq. hydrochloric acid and extracted with EtOAc (3×20 mL). The combined organic layers were dried over sodium sulfate and concentrated to afford the title compound as a brown gum (0.252 g, 91%), which was used in the next step without further purification. Method C HPLC-MS: MH+ requires m/z=236 Found: m/z=236, Rt=0.83 min (82%).

1. temperatureThe mixture was heated to 110 C for 16 h
2. temperatureAfter cooling the residue
3. extractionextracted with EtOAc (3×20 mL)
4. dry with materialThe combined organic layers were dried over sodium sulfate
5. concentrationconcentrated