反应详情

To a solution of 2-{[2-(benzyloxy)-4,6-dimethylpyridin-3-yl]methyl}-8-methyl-1-oxo-1,2,3,4-tetrahydroisoquinoline-7-carboxylic acid (76e, 120 mg, 0.28 mmol), (CH3)2NH.HCl (34 mg, 0.42 mmol) and DIPEA (181 mg, 1.4 mmol) in DMF (5 mL) under N2 atmosphere was added HATU (214 mg, 0.56 mmol). The mixture was stirred at room temperature for 3 hours. The reaction mixture was poured into water (10 mL) and extracted with EtOAc (3×10 mL). The combined organic layers were washed with H2O (10 mL), brine (2×10 mL), dried over Na2SO4, filtered, and concentrated under vacuum. The residue was purified by column chromatography (petroleum ether/EtOAc=1:1) to give 2-{[2-(benzyloxy)-4,6-dimethylpyridin-3-yl]methyl}-N,N,8-trimethyl-1-oxo-1,2,3,4-tetrahydroisoquinoline-7-carboxamide (76f, 80 mg, 63%) as a colorless gum.

1. extractionextracted with EtOAc (3×10 mL)
2. washThe combined organic layers were washed with H2O (10 mL), brine (2×10 mL)
3. dry with materialdried over Na2SO4
4. filtrationfiltered
5. concentrationconcentrated under vacuum
6. customThe residue was purified by column chromatography (petroleum ether/EtOAc=1:1)