反应详情

A flask was charged with 1-cyano-4-hydroxy-7-phenoxy-isoquinoline-3-carboxylic acid (40 mg, 0.13 mmol), HOBt (18 mg, 0.13 mmol) and CH2Cl2 (2 mL). EDC (35 mg, 0.18 mmol) was added, and the mixture was stirred for 10 min. (2R,3S)-3-Amino-2-methyl-butyric acid tert-butyl ester (22 mg, 0.13 mmol) and Hunig's base (0.050 mL, 0.26 mmol) were then added, and the resulting mixture was stirred for 3 days at r.t. Hydrochloric acid (0.1 M) was added to acidify the mixture, and the mixture was extracted with EtOAc. The organic layer was dried over MgSO4 and concentrated. The crude product was purified by column chromatography (0-10% EtOAc/hexanes+2% AcOH) to give 30 mg of the title compound as a white solid. MS: (−) m/z 460.31 (M−1).

1. additionwere then added
2. extractionthe mixture was extracted with EtOAc
3. dry with materialThe organic layer was dried over MgSO4
4. concentrationconcentrated
5. customThe crude product was purified by column chromatography (0-10% EtOAc/hexanes+2% AcOH)