反应详情

To a solution of 1,1-dimethylethyl 3-hydroxy-4,4-bis(methyloxy)-1-piperidinecarboxylate D16 (11 g) in THF (150 ml) was added Potassium t-Butoxide (23.5 g, 210 mmol) at 0° C. The reaction mixture was stirred for 20 mins and the methyliodide (5.2 ml, 84 mmol) was added. The reaction mixture was allowed to warm up to room temperature and stirred overnight. The resulting mixture was concentrated and dissolved in EtOAc and washed with water. The organic layer was concentrated in vacuo to obtain crude product. Product was purified on silica gel eluting with DCM/MeOH 50/1 to obtain the desired product D17 as a yellow oil in 5 g. LCMS [MH+] 298@1.385 min (5 min run)

1. stirringstirred overnight
2. concentrationThe resulting mixture was concentrated
3. dissolutiondissolved in EtOAc
4. washwashed with water
5. concentrationThe organic layer was concentrated in vacuo
6. customto obtain crude product
7. customProduct was purified on silica gel eluting with DCM/MeOH 50/1