[CH:1]12[CH2:9][CH:5]([CH2:6][NH:7][CH2:8]1)[CH2:4][N:3]([C:10]([O:12][CH:13]([CH3:15])[CH3:14])=[O:11])[CH2:2]2.CS(O[CH2:21][CH2:22][C:23]1[CH:28]=[CH:27][C:26]([C:29]#[N:30])=[CH:25][CH:24]=1)(=O)=O.C([O-])([O-])=O.[K+].[K+].N#N>CC#N>[C:29]([C:26]1[CH:27]=[CH:28][C:23]([CH2:22][CH2:21][N:7]2[CH2:8][CH:1]3[CH2:9][CH:5]([CH2:4][N:3]([C:10]([O:12][CH:13]([CH3:15])[CH3:14])=[O:11])[CH2:2]3)[CH2:6]2)=[CH:24][CH:25]=1)#[N:30]iso-Propyl 3,7-diazabicyclo[3.3.1]nonane-3-carboxylate (1.06 g; 5 mmol; see Example H above) was added to a stirred suspension of 4-cyanophenethyl methanesulfonate (1.13 g; 5 mmol; from step (a) above) and K2CO3 (0.96 g; 7 mmol) in MeCN (5 mL) under an inert atmosphere (N2), and the reaction mixture was stirred for 10 h. The solvent was evaporated and the residue partitioned between DCM and NaHCO3 (aq.). The organic layer was separated, dried and concentrated. Purification using column chromatography (DCM:MeOH; 19:1) gave the title compound in a 88% yield.
Wird geladen…