C(OC(=O)[NH:7][CH2:8][C:9](=[O:27])[N:10]1[CH2:14][CH2:13][CH:12]([N:15]2[CH2:20][CH2:19][CH:18]([C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=3)[CH2:17][CH2:16]2)[CH2:11]1)(C)(C)C.C(O)(C(F)(F)F)=O.C1(C)C=CC=CC=1>C(Cl)Cl>[NH2:7][CH2:8][C:9]([N:10]1[CH2:14][CH2:13][CH:12]([N:15]2[CH2:16][CH2:17][CH:18]([C:21]3[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=3)[CH2:19][CH2:20]2)[CH2:11]1)=[O:27]To a solution of {2-oxo-2-[3-(4-phenyl-piperidin-1-yl)-pyrrolidin-1-yl]-ethyl}-carbamic acid tert-butyl ester (preparation #10) (3.25 g, 8.39 mmol) in DCM (200 mL) was added TFA (15 mL). The reaction mixture was stirred at ambient temperature for about 5 h. Toluene (100 mL) was added and the solvents were removed in vacuo. The residue was dissolved in DCM (400 mL) and the organic was washed with saturated NaHCO3, 1.0N NaOH, brine, dried over MgSO4, filtered and concentrated in vacuo to give 2-amino-1-[3-(4-phenyl-piperidin-1-yl)-pyrrolidin-1-yl]-ethanone (2.34 g, 97%) as a light tan solid; RP-HPLC (Table 1, Method a) Rt 1.09 min; m/z: (M+H)+ 288.
Wird geladen…
