反应详情

温度

-78 °C

A mixture of THF (160 mL) and diisopropyl amine (9.92 mL, 70.8 mmol, 1.2 eq) was cooled to −78° C. and a 2.5 M solution of n-BuLi in heptanes (28.3 mL, 70.8 mmol, 1.2 eq) was added slowly. The solution was stirred for 15 min, warmed to 0° C. for 20 min and cooled back to −78° C. Ethyl N-Bocpiperidine-4-carboxylate (11 mL, 59 mmol, 1 eq.) in 10 mL of THF was added drop-wise and stirred for 40 min before it was warmed to rt. The reaction mixture was stirred for 12 h, transferred to a separatory funnel, quenched with 500 mL of water and extracted with ethyl acetate (2×300 mL). The combined organics were dried over Na2SO4 and concentrated under vacuum to give the title compound as a yellow oil (13.9 g, 76%).

1. temperaturewarmed to 0° C. for 20 min
2. temperaturecooled back to −78° C
3. stirringstirred for 40 min before it
4. temperaturewas warmed to rt
5. stirringThe reaction mixture was stirred for 12 h
6. customtransferred to a separatory funnel
7. customquenched with 500 mL of water
8. extractionextracted with ethyl acetate (2×300 mL)
9. dry with materialThe combined organics were dried over Na2SO4
10. concentrationconcentrated under vacuum