C([C:3]1([O:16][Si:17]([CH3:20])([CH3:19])[CH3:18])[CH2:8][CH2:7][CH2:6][N:5](C(OC(C)(C)C)=O)[CH2:4]1)#N.Cl.[C:22](=[O:25])([O-])[O-:23].[Cs+].[Cs+].[Si](Cl)(C)(C)[CH3:29]>CO>[CH3:18][Si:17]([CH3:19])([CH3:20])[O:16][C:3]1([C:22]([O:23][CH3:29])=[O:25])[CH2:8][CH2:7][CH2:6][NH:5][CH2:4]1
tert-Butyl 3-cyano-3-(trimethylsilyloxy)piperidine-1-carboxylate, Preparation 34A (170 mg, 0.570 mmol) was treated with 6N HCl in MeOH (10 mL) at 80° C. for 12 hours. Solvents were removed in vacuo and the resulting material was dissolved in MeOH (10 mL). HCl (g) was bubbled through the mixture for 15 minutes. The solids were concentrated in vacuo. The residue was dissolved in DCM (10.00 mL) and cesium carbonate (928 mg, 2.85 mmol) was added. Next, TMS—Cl (0.146 mL, 1.139 mmol) was added and the mixture was stirred for 1 hour. The mixture was filtered and the solids were concentrated in vacuo and taken to the next step without further purification.
Wird geladen…
