反应详情

温度

-78 °C

To a solution of benzyl 3-oxopiperidine-1-carboxylate (2.33 g, 10 mmol) in dry THF (50 mL) at −78° C. was added MeMgBr (3.6 mL, 3M solution in THF, 11 mmol) slowly. The reaction was allowed to stir at −78° C. for 10 min then slowly warmed to r.t. The reaction was quenched with NH4Cl and dissolved in EtOAc (300 mL) and washed with saturated NH4Cl and brine, dried and filtered, and concentrated to give the crude. The crude material was further purified by silica gel chromatography to yield benzyl 3-hydroxy-3-methylpiperidine-1-carboxylate. (53% yield). LCMS (m/z): 250.1 (MH+); LC Rt=2.98 min.

1. temperaturethen slowly warmed to r.t
2. customThe reaction was quenched with NH4Cl
3. dissolutiondissolved in EtOAc (300 mL)
4. washwashed with saturated NH4Cl and brine
5. customdried
6. filtrationfiltered
7. concentrationconcentrated
8. customto give the crude
9. customThe crude material was further purified by silica gel chromatography