反应详情

To a solution of 1,1-dimethylethyl 3,4,4-tris(methyloxy)-1-piperidinecarboxylate D17 (4.85 g) in HCl/1,4-Dioxane (50 mL) was heated at 50° C. and stirred overnight. Water (50 ml) was added to the reaction mixture and the pH adjusted to 10.0 using sodium hydroxide. After that BOC anhydride (4.22 g, 19.4 mmol) was added to the reaction mixture and stirred for 4 hours. The resulting mixture was extracted with EtOAc (3×100 ml). The organic layer was dried over anhydrous MgSO4, concentrated in vacuo to afford the desired product D18 in 3.1 g. LCMS [M-55]=174@1.29 min (5 min run)

1. stirringstirred for 4 hours
2. extractionThe resulting mixture was extracted with EtOAc (3×100 ml)
3. dry with materialThe organic layer was dried over anhydrous MgSO4
4. concentrationconcentrated in vacuo