反应详情

温度

-55 °C

To a solution of 1-tert-butyl 3-ethyl piperidine-1,3-dicarboxylate (2.6 g, 10.0 mmol) in THF (30 mL) was slowly added LDA (6.7 mL, 12.0 mmol, 1.8 M solution in heptane-/tetrahydrofuran/ethylbenzene) at −78° C. and the mixture was slowly warmed to −55° C. over 1 h. To this mixture, 1-bromo-3-methyl-2-butene (1.55 g, 10.5 mmol) was slowly added and the reaction was warmed to room temperature and stirred for 4 h. The mixture was quenched with saturated NH4Cl and extracted with diethyl ether, and the combined extracts were washed with brine, dried and concentrated. The product (2.75 g, 85%) was purified by CombiFlash eluted with hexane/ethyl acetate.

1. customat −78° C.
2. temperaturethe reaction was warmed to room temperature
3. customThe mixture was quenched with saturated NH4Cl
4. extractionextracted with diethyl ether
5. washthe combined extracts were washed with brine
6. customdried
7. concentrationconcentrated
8. customThe product (2.75 g, 85%) was purified by CombiFlash
9. washeluted with hexane/ethyl acetate