反应详情

To a solution of 3-methyl 1-(phenylmethyl) (3S,6R)-6-methyl-1,3-piperidinedicarboxylate (15 g, 51.5 mmol) in THF/water/CH3OH (10/5/1, 480 mL) was added LiOH.H2O (2.59 g, 61.8 mmol), and the reaction mixture was stirred at room temperature for about 1 hour. The mixture was acidified with 1N HCl until the pH was ˜5, and then concentrated in vacuo. The resulting residue was extracted with EtOAc (2×300 mL) and CHCl3 (2×300 mL), and the combined organic layers were dried (MgSO4), filtered and concentrated in vacuo to afford the crude title compound (17 g). LC-MS (ES) m/z=278 [M+H]+.

1. concentrationconcentrated in vacuo
2. extractionThe resulting residue was extracted with EtOAc (2×300 mL) and CHCl3 (2×300 mL)
3. dry with materialthe combined organic layers were dried (MgSO4)
4. filtrationfiltered
5. concentrationconcentrated in vacuo