反应详情

To a solution of 3-[(1-{[(1,1-dimethylethyl)oxy]carbonyl}-4-piperidinyl)methyl]benzoic acid (128 mg, 0.40 mmol) in CHCl3 (2.0 mL) was added 1,1-dimethylethyl (2S)-4-({3-[5-(aminomethyl)-2-thienyl]phenyl)methyl)-2-methyl-1-piperazinecarboxylate (160 mg, 0.40 mmol), TEA (0.1 ml, 0.7 mmol), EDC (115 mg, 0.6 mmol) and HOBt (59 mg, 0.44 mmol). The reaction mixture was stirred at room temperature for 2 h, followed by addition of 0.5 mL of saturated Na2CO3. The organic layer was isolated via a hydrophobic frit followed by addition of 0.5 mL of TFA, and stirred at room temperature for 1 h. After removal of the solvent, the residue was purified by Gilson reverse phase HPLC, eluting with acetonitrile/water/0.1% TFA (10/90 to 70/30, v/v, over 12 min), to give the title compound (100 mg, 50%). LC/MS: m/z, 503 (M+H), 1.22 min.

1. customThe organic layer was isolated via a hydrophobic frit
2. stirringstirred at room temperature for 1 h
3. customAfter removal of the solvent
4. customthe residue was purified by Gilson reverse phase HPLC
5. washeluting with acetonitrile/water/0.1% TFA (10/90 to 70/30, v/v, over 12 min)