反应详情

温度

0 °C

tert-Butyl 4-cyano-4-pyridin-2-ylpiperidine-1-carboxylate (I-2) (5.45 g, 19 mmole) was dissolved in TFA-DCM (1:1, 50 mL) at 0° C. The resultant reaction mixture was stirred for 40 min at 0° C. After this time, LCMS indicated that the reaction was completion. The reaction mixture solution was concentrated. The residue was treated with 2N NaOH-brine (1: 1, 80 mL) and extracted with EtOAc (5×200 mL). The combined EtOAc extracts were washed with brine, dried over MgSO4, filtered, concentrated to afford the desired product 4-pyridin-2-ylpiperidine4-carbonitrile (I-3) as a yellow solid. Analytical LCMS: single peak (214 nm), 0.962 min. This product was used in next step without further purification.

1. customThe resultant reaction mixture
2. concentrationThe reaction mixture solution was concentrated
3. additionThe residue was treated with 2N NaOH-brine (1: 1, 80 mL)
4. extractionextracted with EtOAc (5×200 mL)
5. washThe combined EtOAc extracts were washed with brine
6. dry with materialdried over MgSO4
7. filtrationfiltered
8. concentrationconcentrated