反应详情

温度

150 °C

A mixture of 1-cyano-4-hydroxy-7-phenyl-isoquinoline-3-carboxylic acid methyl ester (47 mg, 0.15 mmol), 3-amino-2,2-dimethyl-propionic acid TFA salt (143 mg, 0.62 mmol) and NaOMe (67 mg, 1.24 mmol) in EtOH (3 mL) was heated at 150° C. in a microwave reactor for 2 h. The solvent was evaporated, and the residue was partitioned between water (30 mL) and EtOAc (30 mL). 1 M HCl was added with vigorous stirring until pH was ˜2. The organic layer was dried over MgSO4 and concentrated. The crude product was purified by column chromatography (0-25% EtOAc/hexanes+2% AcOH) to give 36 mg of the title compound as a light brown solid. MS: (−) m/z 388.13 (M−1).

1. customThe solvent was evaporated
2. customthe residue was partitioned between water (30 mL) and EtOAc (30 mL)
3. addition1 M HCl was added
4. dry with materialThe organic layer was dried over MgSO4
5. concentrationconcentrated
6. customThe crude product was purified by column chromatography (0-25% EtOAc/hexanes+2% AcOH)