反应详情

To a mixture of 4′-methyl-5-(methylsulfonyl)biphenyl-3-carboxylic acid (35 mg, 0.12 mmol), N-(3-dimethylaminopropyl)-N′-ethylcarbodiimide hydrochloride (46 mg, 0.24 mmol), 1-hydroxybenzotriazole hydrate (18 mg, 0.12 mmol), and CH2Cl2 (3 mL) were added (S)-2-(tert-butyldimethylsilyloxy)-1-(2-methylpyrimidin-5-yl)ethanamine (48 mg, 0.18 mmol) (WO 2008/130481) and N,N-diisopropylethylamine (42 μL, 0.24 mmol). The mixture was stirred at room temperature overnight and then concentrated. The residue was dissolved in MeOH (5 mL) and concentrated HCl solution (0.5 mL) was added. The mixture was stirred at room temperature for 2 h and then concentrated in vacuo. The residue was purified by preparative HPLC (100×20.2 mm, C18 column; 30-80% MeCN-water[10 mM Et2NH]) to afford a white solid.

1. concentrationconcentrated
2. dissolutionThe residue was dissolved in MeOH (5 mL)
3. additionconcentrated HCl solution (0.5 mL) was added
4. stirringThe mixture was stirred at room temperature for 2 h
5. concentrationconcentrated in vacuo
6. customThe residue was purified by preparative HPLC (100×20.2 mm, C18 column; 30-80% MeCN-water[10 mM Et2NH])
7. customto afford a white solid