反应详情

To a solution of 1,1-dimethylethyl 3-(methyloxy)-4-oxo-1-piperidinecarboxylate D18 (2.9 g) in MeOH (100 ml), was added sodium cyanoborohydride (7.9 g, 126 mmol) and ammonium acetate (9.7 g, 126 mmol) at R.T. The reaction mixture was stirred for 4 hours. The resulting mixture was concentrated in vacuo, dissolved in water, basified with sodium hydroxide to pH10 and extracted with DCM. The organic layer was dried over anhydrous MgSO4, concentrated in vacuo to get the desired product D19 in 2.85 g. LCMS [MH+] 231@0.83 min (5 min run)

1. concentrationThe resulting mixture was concentrated in vacuo
2. dissolutiondissolved in water
3. extractionextracted with DCM
4. dry with materialThe organic layer was dried over anhydrous MgSO4
5. concentrationconcentrated in vacuo