[C:1]([O:5][C:6]([NH:8][CH2:9][C:10]([OH:12])=O)=[O:7])([CH3:4])([CH3:3])[CH3:2].C1CN([P+](ON2N=NC3C=CC=CC2=3)(N2CCCC2)N2CCCC2)CC1.F[P-](F)(F)(F)(F)F.[NH2:46][C:47]1[C:56]2[C:51](=[CH:52][CH:53]=[C:54]([O:57][CH2:58][C:59]3[CH:64]=[CH:63][CH:62]=[CH:61][CH:60]=3)[CH:55]=2)[CH:50]=[CH:49][CH:48]=1.C(N(CC)C(C)C)(C)C>C(Cl)Cl>[CH2:58]([O:57][C:54]1[CH:55]=[C:56]2[C:51]([CH:50]=[CH:49][CH:48]=[C:47]2[NH:46][C:10](=[O:12])[CH2:9][NH:8][C:6]([O:5][C:1]([CH3:2])([CH3:3])[CH3:4])=[O:7])=[CH:52][CH:53]=1)[C:59]1[CH:60]=[CH:61][CH:62]=[CH:63][CH:64]=1To N-(tert-butoxycarbonyl)glycine (527 mg, 3.01 mmol) in dry CH2Cl2 (5 mL) under argon were added PYBOP (1.65 g, 3.16 mmol), 1-amino-7-benzyloxynaphthalene, as described above in Step J, (750 mg, 3.01 mmol), and N,N-diisopropylethylamine (0.55 mL, 3.16 mmol). The reaction mixture was stirred for 18 hrs, then partitioned between CH2Cl2 (200 mL) and 10% aqueous citric acid (50 mL). The organic layer was dried over Na2SO4, filtered, and concentrated in vacuo. The crude product was sufficiently pure for use in the next reaction.
Wird geladen…