反应详情

To a solution of 3-[(1-{[(1,1-dimethylethyl)oxy]carbonyl}-4-piperidinyl)methyl]benzoic acid (108 mg, 0.34 mmol) in dry DMF (2 mL) was added phenylmethyl (2S)-4-{[5′-(aminomethyl)-2′-fluoro-3-biphenylyl]methyl}-2-methyl-1-piperazinecarboxylate (150 mg, 0.334 mmol), DIPEA (0.1 mL, 0.7 mmol), HATU (142 mg, 0.37 mmol) and HOBt (150 mg, 1.1 mmol). The reaction mixture was stirred at room temperature for 2 h, followed by addition of saturated aq. Na2CO3 (1 mL) and EtOAc (5 mL). The organic layer was separated, dried over Na2SO4, and filtered. The filtrate was concentrated and the residue was purified on a 5 g amminopropyl SPE cartridge, eluting with DCM (3×5 mL), EtOAc (3×5 mL), and MeOH (3×5 mL). The product was recovered after evaporation of the DCM fractions (130 mg, 80%). LC/MS: m/z, 749 (M+H), 2.32 min.

1. customThe organic layer was separated
2. dry with materialdried over Na2SO4
3. filtrationfiltered
4. concentrationThe filtrate was concentrated
5. customthe residue was purified on a 5 g amminopropyl SPE cartridge
6. washeluting with DCM (3×5 mL), EtOAc (3×5 mL), and MeOH (3×5 mL)
7. customThe product was recovered
8. customafter evaporation of the DCM fractions (130 mg, 80%)
9. customm/z, 749 (M+H), 2.32 min.